CN109225267A - A kind of vanadium disulfide nanometer stick array elctro-catalyst and preparation method thereof - Google Patents
A kind of vanadium disulfide nanometer stick array elctro-catalyst and preparation method thereof Download PDFInfo
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- CN109225267A CN109225267A CN201811266185.5A CN201811266185A CN109225267A CN 109225267 A CN109225267 A CN 109225267A CN 201811266185 A CN201811266185 A CN 201811266185A CN 109225267 A CN109225267 A CN 109225267A
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- carbon cloth
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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
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- C—CHEMISTRY; METALLURGY
- C25—ELECTROLYTIC OR ELECTROPHORETIC PROCESSES; APPARATUS THEREFOR
- C25B—ELECTROLYTIC OR ELECTROPHORETIC PROCESSES FOR THE PRODUCTION OF COMPOUNDS OR NON-METALS; APPARATUS THEREFOR
- C25B1/00—Electrolytic production of inorganic compounds or non-metals
- C25B1/01—Products
- C25B1/02—Hydrogen or oxygen
- C25B1/04—Hydrogen or oxygen by electrolysis of water
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- C—CHEMISTRY; METALLURGY
- C25—ELECTROLYTIC OR ELECTROPHORETIC PROCESSES; APPARATUS THEREFOR
- C25B—ELECTROLYTIC OR ELECTROPHORETIC PROCESSES FOR THE PRODUCTION OF COMPOUNDS OR NON-METALS; APPARATUS THEREFOR
- C25B11/00—Electrodes; Manufacture thereof not otherwise provided for
- C25B11/04—Electrodes; Manufacture thereof not otherwise provided for characterised by the material
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- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02E—REDUCTION OF GREENHOUSE GAS [GHG] EMISSIONS, RELATED TO ENERGY GENERATION, TRANSMISSION OR DISTRIBUTION
- Y02E60/00—Enabling technologies; Technologies with a potential or indirect contribution to GHG emissions mitigation
- Y02E60/30—Hydrogen technology
- Y02E60/36—Hydrogen production from non-carbon containing sources, e.g. by water electrolysis
Abstract
The present invention provides a kind of vanadium disulfide nanometer stick array elctro-catalyst, preparation methods are as follows: carbon-based is immersed in NaVO for conductive3: CH3CSNH2: C6H12N4Mass ratio is (0.1 ~ 0.5) (0.2 ~ 0.8): in the solution of (0.5 ~ 1.5), hydro-thermal reaction obtains uniform nano bar-shape VS2.The present invention has low synthesis temperature, and simple process is easy to operate, and raw material is cheap and easy to get, at low cost, and yield is high, is not necessarily to post-processing, environmentally friendly, can be suitble to be mass produced；The product chemistry composition of preparation 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 10mA/cm2, overpotential is about 206mV.
Description
Technical field
The invention belongs to electrolysis water catalyst technical fields, and in particular to a kind of vanadium disulfide nanometer stick array elctro-catalyst and
Preparation method.
Background technique
Electrocatalytic decomposition water technology is to be now widely used for one of industrial production system since its process equipment is simple
The method of standby hydrogen, it is the one of the most potential technology for developing sustainable clean energy resource and scientific research field research
A important directions.The platinum groups noble metal such as Pt, Pd is the catalyst of presently found best electrolysis elutriation ammonia, but due to its valence
The reasons such as lattice are expensive, earth reserves are low, easily poison, make it difficult to be widely used in large-scale industrial production, because
And finding alternative electrolysis water catalyst becomes an important topic in this field.Studies have shown that vanadium valence state flexibly (+
3 ,+4 ,+5), there is good reactivity, in addition, charge biography can be effectively facilitated by catalyst in conjunction with conductive substrates
It is defeated, and can significantly enhance its catalytic activity and stability.
This patent uses efficient, simple and inexpensive one step hydro thermal method, is prepared for vanadium disulfide in carbon cloth substrate and receives
Rice stick array, effectively improves electric conductivity, to improve electrolysis water Hydrogen Evolution Performance.
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 vanadium disulfide nanometer stick array catalyst
Preparation method, this method is easy to operate, and reaction condition is mild, and time-consuming short, the vanadium disulfide product purity of preparation is high, pattern and
Size uniformity, and electrocatalytic hydrogen evolution performance is more excellent.
To achieve the goals above, the present invention uses following technical scheme.
(1) carbon cloth is cut into the rectangle of 1 × 5cm, activates 1 ~ 3 hour in 80 ~ 120 DEG C of reflux, then with ethyl alcohol and
Deionized water is respectively washed at 3 ~ 5 times, 40 ~ 70 DEG C dry 6 ~ 8h carbon cloth that obtains that treated；
(2) (0.1g ~ 0.5g) NaVO is weighed respectively3、(0.2g~0.8g) CH3CSNH2(0.5g ~ 1.5g) C6H12N4, it is dissolved in
In 20 ~ 40ml deionized water, 40 ~ 60min of magnetic agitation, obtains clear solution at room temperature；
(3) carbon cloth that (1) is handled is put into reaction liner, the clear solution that (2) obtain is poured into, it is anti-that sealing carries out hydro-thermal
It answers, sets reaction temperature as 160 ~ 220 DEG C, the reaction time is 18 ~ 30h；
(4) after reaction, to reaction kettle cooled to room temperature, carbon cloth is taken out, it is then clear with ethyl alcohol and deionized water difference
Wash 3 times, finally will at 40 ~ 70 DEG C of carbon cloth dry 5 ~ 8h to get arriving uniform nano bar-shape VS2。
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 process is easy to operate, and raw material is cheap and easy to get, at low cost, and yield is high, is not necessarily to post-processing, environmentally friendly, can be suitble to big
Large-scale production；
(3) the product chemistry composition of this method preparation is uniform, and purity is high, pattern is uniform, energy when being used as electrolysis water electrode material
Excellent chemical property is enough shown, in 10mA/cm2Current density under, overpotential is about 206mV.
Detailed description of the invention
Fig. 1 is the VS being grown on carbon cloth prepared by the embodiment of the present invention 32The X-ray diffraction (XRD) of nanometer stick array
Map；
Fig. 2 is the VS being grown on carbon cloth prepared by the embodiment of the present invention 32Scanning electron microscope (SEM) photo of nanometer stick array；
Fig. 3 is the VS being grown on carbon cloth prepared by the embodiment of the present invention 32Linear sweep voltammetry (LSV) property of nanometer stick array
It can test chart.
Specific embodiment
With reference to the accompanying drawing and embodiment invention is further described in detail:
Embodiment 1:
(1) carbon cloth is cut into the rectangle of 1 × 5cm, 80 ~ 120 DEG C of reflux activation 1 ~ 3 hours in concentrated nitric acid, is then used
Ethyl alcohol and deionized water are respectively washed at 3 times, 50 DEG C the dry 8h carbon cloth that obtains that treated；
(2) 0.1g NaVO is weighed respectively3, 0.2g TAA(CH3CSNH2) and 0.5g C6H12N4, it is dissolved in 20ml deionized water,
Magnetic agitation 40min at room temperature obtains clear solution；
(3) carbon cloth that (1) is handled is put into reaction liner, the clear solution that (2) obtain is poured into, it is anti-that sealing carries out hydro-thermal
It answers, sets reaction temperature as 160 DEG C, reaction time 18h；
(4) after reaction, to reaction kettle cooled to room temperature, carbon cloth is taken out, it is then clear with ethyl alcohol and deionized water difference
Wash 3 times, finally will at 50 DEG C of carbon cloth dry 8h to get arriving uniform nano bar-shape VS2。
Embodiment 2:
(1) carbon cloth is cut into the rectangle of 1 × 5cm, 80 DEG C of reflux activation 2 hours in concentrated nitric acid, then with ethyl alcohol and
Deionized water is respectively washed at 4 times, 50 DEG C the dry 8h carbon cloth that obtains that treated；
(2) 0.3g NaVO is weighed respectively3, 0.9g TAA(CH3CSNH2) and 0.8g C6H12N4, it is dissolved in 30ml deionized water,
Magnetic agitation 40min at room temperature obtains clear solution；
(3) carbon cloth that (1) is handled is put into reaction liner, the clear solution that (2) obtain is poured into, it is anti-that sealing carries out hydro-thermal
It answers, sets reaction temperature as 200 DEG C, reaction time 22h；
(4) after reaction, to reaction kettle cooled to room temperature, carbon cloth is taken out, it is then clear with ethyl alcohol and deionized water difference
Wash 3 times, finally will at 50 DEG C of carbon cloth dry 8h to get arriving uniform nano bar-shape VS2。
Embodiment 3:
(1) carbon cloth is cut into the rectangle of 1 × 5cm, 80 DEG C of reflux activation 2 hours in concentrated nitric acid, then with ethyl alcohol and
Deionized water is respectively washed at 5 times, 60 DEG C the dry 7h carbon cloth that obtains that treated；
(2) 0.4g NaVO is weighed respectively3, 1.2g TAA(CH3CSNH2) and 1.2g C6H12N4, it is dissolved in 35ml deionized water,
Magnetic agitation 60min at room temperature obtains clear solution；
(3) carbon cloth that (1) is handled is put into reaction liner, the clear solution that (2) obtain is poured into, it is anti-that sealing carries out hydro-thermal
It answers, sets reaction temperature as 180 DEG C, the reaction time is for 24 hours；
(4) after reaction, to reaction kettle cooled to room temperature, carbon cloth is taken out, it is then clear with ethyl alcohol and deionized water difference
Wash 3 times, finally will at 60 DEG C of carbon cloth dry 7h to get arriving uniform nano bar-shape VS2。
Fig. 1 is the VS manufactured in the present embodiment being grown on carbon cloth2X-ray diffraction (XRD) map of nanometer stick array.
Characteristic peak and VS in figure, in XRD test result2Characteristic peak it is consistent, illustrate the present invention VS has been grown on carbon-based2。
Fig. 2 is the VS being grown on carbon cloth prepared by the embodiment of the present invention 32The scanning electron microscope (SEM) of nanometer stick array is shone
Piece.SEM photograph shows, the VS that the present invention is grown on carbon-based2Pattern with irregular nanometer stick array.
Fig. 3 is the VS being grown on carbon cloth prepared by the embodiment of the present invention 32The linear sweep voltammetry of nanometer stick array
(LSV) performance test figure.LSV performance test is shown, in 50mA/cm2Current density under, overpotential is about 509mV；?
100mA/cm2Current density under, overpotential is about 583mV.
Embodiment 4:
(1) carbon cloth is cut into the rectangle of 1 × 5cm, 100 DEG C of reflux activation 1 hours in concentrated nitric acid, then with ethyl alcohol and
Deionized water is respectively washed at 4 times, 70 DEG C the dry 6h carbon cloth that obtains that treated；
(2) 0.5g NaVO is weighed respectively3, 0.8g TAA(CH3CSNH2) and 1.5g C6H12N4, it is dissolved in 40ml deionized water,
Magnetic agitation 60min at room temperature obtains clear solution；
(3) carbon cloth that (1) is handled is put into reaction liner, the clear solution that (2) obtain is poured into, it is anti-that sealing carries out hydro-thermal
It answers, sets reaction temperature as 220 DEG C, reaction time 28h；
(4) after reaction, to reaction kettle cooled to room temperature, carbon cloth is taken out, it is then clear with ethyl alcohol and deionized water difference
Wash 3 times, finally will at 70 DEG C of carbon cloth dry 6h to get arriving uniform nano bar-shape VS2。
Claims (6)
1. a kind of preparation method of vanadium disulfide nanometer stick array elctro-catalyst, which comprises the following steps:
Carbon-based NaVO is immersed in for conductive3: CH3CSNH2: C6H12N4Mass ratio is (0.1 ~ 0.5) (0.2 ~ 0.8): (0.5 ~ 1.5)
In solution, hydro-thermal reaction obtains uniform nano bar-shape VS2。
2. a kind of preparation method of vanadium disulfide nanometer stick array elctro-catalyst according to claim 1, which is characterized in that
The carbon-based carbon cloth for activated processing of the conduction.
3. a kind of preparation method of vanadium disulfide nanometer stick array elctro-catalyst according to claim 1, which is characterized in that
The carbon cloth of the activated processing is obtained by method comprising the following steps: carbon cloth being flowed back in concentrated nitric acid at 80 ~ 120 DEG C and is lived
Change 1 ~ 3 hour, is then respectively washed at 3 ~ 5 times, 40 ~ 70 DEG C dry 6 ~ 8h carbon that obtains that treated with ethyl alcohol and deionized water
Cloth.
4. a kind of preparation method of vanadium disulfide nanometer stick array elctro-catalyst according to claim 1, which is characterized in that
The hydrothermal temperature is 160 ~ 220 DEG C, and the hydro-thermal reaction time is 18 ~ 30h.
5. a kind of preparation method of vanadium disulfide nanometer stick array elctro-catalyst according to claim 1, which is characterized in that
Specific steps include:
1) carbon cloth is cut into the rectangle of 1 × 5cm, 80 ~ 120 DEG C of reflux activation 1 ~ 3 hours in concentrated nitric acid, then uses second
Pure and mild deionized water is respectively washed at 3 ~ 5 times, 40 ~ 70 DEG C dry 6 ~ 8h carbon cloth that obtains that treated；
2) NaVO of 0.1g ~ 0.5g is weighed respectively3, 0.2g ~ 0.8g CH3CSNH2And the C of 0.5g ~ 1.5g6H12N4, it is dissolved in 20 ~
In 40ml deionized water, 40 ~ 60min of magnetic agitation, obtains clear solution at room temperature；
3) carbon cloth of step 1) processing is put into reaction liner, the clear solution that step 2 is obtained pours into, and sealing carries out water
Thermal response sets reaction temperature as 160 ~ 220 DEG C, and the reaction time is 18 ~ 30h；
4) after reaction, to reaction kettle cooled to room temperature, carbon cloth is taken out, is then respectively washed with ethyl alcohol and deionized water
3 times, finally will at 40 ~ 70 DEG C of carbon cloth dry 5 ~ 8h to get arriving uniform nano bar-shape VS2。
6. a kind of vanadium disulfide nanometer stick array elctro-catalyst of any one of claim 1 ~ 4 the method preparation.
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Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| 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 |
| 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 |
| CN110396598A (en) * | 2019-07-22 | 2019-11-01 | 广东环境保护工程职业学院 | A kind of method that waste and old lithium ion battery manganate cathode material for lithium recycles |
| CN114142048A (en) * | 2021-11-30 | 2022-03-04 | 成都先进金属材料产业技术研究院股份有限公司 | Electrode modification method for vanadium cell |
| CN114142043A (en) * | 2021-11-30 | 2022-03-04 | 成都先进金属材料产业技术研究院股份有限公司 | Method for improving electrochemical performance of electrode for vanadium battery |
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| CN105600770A (en) * | 2016-02-06 | 2016-05-25 | 陕西科技大学 | Preparation method and application of carbon fiber reinforced polymer-based composite material |
| CN107902697A (en) * | 2017-11-02 | 2018-04-13 | 陕西科技大学 | A kind of nanometer sheet self assembled three-dimensional VS of (001) orientation2Micron bar and preparation method thereof |
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| CN105600770A (en) * | 2016-02-06 | 2016-05-25 | 陕西科技大学 | Preparation method and application of carbon fiber reinforced polymer-based composite material |
| CN107902697A (en) * | 2017-11-02 | 2018-04-13 | 陕西科技大学 | A kind of nanometer sheet self assembled three-dimensional VS of (001) orientation2Micron bar and preparation method thereof |
Cited By (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| 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 |
| 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 |
| CN110396598A (en) * | 2019-07-22 | 2019-11-01 | 广东环境保护工程职业学院 | A kind of method that waste and old lithium ion battery manganate cathode material for lithium recycles |
| CN114142048A (en) * | 2021-11-30 | 2022-03-04 | 成都先进金属材料产业技术研究院股份有限公司 | Electrode modification method for vanadium cell |
| CN114142043A (en) * | 2021-11-30 | 2022-03-04 | 成都先进金属材料产业技术研究院股份有限公司 | Method for improving electrochemical performance of electrode for vanadium battery |
| CN114142048B (en) * | 2021-11-30 | 2023-10-27 | 成都先进金属材料产业技术研究院股份有限公司 | Electrode modification method for vanadium battery |
| CN114142043B (en) * | 2021-11-30 | 2023-10-27 | 成都先进金属材料产业技术研究院股份有限公司 | Method for improving electrochemical performance of electrode for vanadium battery |
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