CN109650493A - A kind of VS with hierarchical structure2The synthetic method of nano-chip arrays electrode material - Google Patents

A kind of VS with hierarchical structure2The synthetic method of nano-chip arrays electrode material Download PDF

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CN109650493A
CN109650493A CN201910058479.7A CN201910058479A CN109650493A CN 109650493 A CN109650493 A CN 109650493A CN 201910058479 A CN201910058479 A CN 201910058479A CN 109650493 A CN109650493 A CN 109650493A
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nano
electrode material
chip arrays
reaction
hierarchical structure
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CN109650493B (en
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曹丽云
施潇虎
冯亮亮
黄剑锋
李振哲
刘明鑫
陈倩
杨立学
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Shaanxi University of Science and Technology
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    • C—CHEMISTRY; METALLURGY
    • C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
    • C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
    • C02F1/00—Treatment of water, waste water, or sewage
    • C02F1/46—Treatment of water, waste water, or sewage by electrochemical methods
    • C02F1/461—Treatment of water, waste water, or sewage by electrochemical methods by electrolysis
    • C02F1/46104—Devices therefor; Their operating or servicing
    • C02F1/46109—Electrodes
    • C—CHEMISTRY; METALLURGY
    • C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
    • C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
    • C02F1/00—Treatment of water, waste water, or sewage
    • C02F1/46—Treatment of water, waste water, or sewage by electrochemical methods
    • C02F1/461—Treatment of water, waste water, or sewage by electrochemical methods by electrolysis
    • C02F1/46104—Devices therefor; Their operating or servicing
    • C02F1/46109—Electrodes
    • C02F2001/46133—Electrodes characterised by the material

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  • Chemical & Material Sciences (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • Electrochemistry (AREA)
  • General Chemical & Material Sciences (AREA)
  • Life Sciences & Earth Sciences (AREA)
  • Hydrology & Water Resources (AREA)
  • Engineering & Computer Science (AREA)
  • Environmental & Geological Engineering (AREA)
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  • Electrodes For Compound Or Non-Metal Manufacture (AREA)

Abstract

A kind of VS with hierarchical structure2The synthetic method of nano-chip arrays electrode material is handled carbon cloth using electrochemistry anodic oxidation；Then deionized water is added in vanadium source and sulphur source under stiring and obtains suspension A；Dodecyldimethylamine oxide is added in suspension A and stirs evenly to obtain solution B；Solution B and the carbon cloth handled well are fitted into autoclave, is subsequently placed in reaction baking oven and carries out hydro-thermal reaction；To which after reaction, reaction kettle is cooled to room temperature, product deionized water and ethyl alcohol alternately rinse to be dried in vacuo afterwards for several times and obtain the VS with hierarchical structure2Nano-chip arrays electrode material.The present invention uses efficient, simple and inexpensive one step hydro thermal method, and vanadium disulfide nano-chip arrays elctro-catalyst is prepared on carbon cloth, electrolysis water Hydrogen Evolution Performance is effectively promoted.

Description

A kind of VS with hierarchical structure2The synthetic method of nano-chip arrays electrode material
Technical field
The invention belongs to electrolysis water catalytic fields, are related to a kind of preparation of electrolysis water catalytic electrode material, and in particular to one Kind has the VS of hierarchical structure2The synthetic method of nano-chip arrays electrode material.
Background technique
It is big to the demand of the energy, waste is serious, fossil fuel with the growth of population in the world and the fast development of economy A series of problems such as exhaustion, carbon emission, greenhouse effects are forcing the whole world to carry out primary thorough energy revolution.It was verified that Energy resource structure based on fossil fuel increasingly can not meet the requirement of human social development.Therefore, find cleaning, efficiently, can The renewable sources of energy and energy carrier become the focus of today's society discussion and research.Green sustainable energy of the Hydrogen Energy as a new generation Source, people place high hopes to it.Electrocatalytic decomposition water technology is one of effective way of hydrogen manufacturing.
Transient metal sulfide has many advantages, such as rich content, low in cost, has in terms of electro-catalysis water-splitting extensive Application prospect.Wherein, VS2The intrinsic metallic character of material and cheap advantage receive the extensive concern of people.Studies have shown that The valence state of vanadium flexibly (+3 ,+4 ,+5), has good reactivity, in addition, by catalyst in conjunction with conductive substrates, Ke Yiyou Effect ground promotes charge transmission, and can significantly enhance its catalytic activity and stability.
Summary of the invention
The purpose of the present invention is to provide a kind of VS with hierarchical structure2The synthesis side of nano-chip arrays electrode material Method, this method is easy to operate, and reaction condition is mild, time-consuming short, low in cost, and the vanadium disulfide product purity of preparation is high, pattern And size uniformity, and electrocatalytic hydrogen evolution is had excellent performance.
In order to achieve the above objectives, the technical solution adopted by the present invention is that:
1) carbon cloth being handled using electrochemistry anodic oxidation, selected electrolyte is that concentration is 3~5mol/L ammonium dihydrogen phosphate, Faradaic current is 0.2~0.6A, is then dried in vacuo；
2) by 1:(3~6) molar ratio take vanadium source and sulphur source, 25ml-40ml is added in vanadium source and sulphur source under stiring and is gone The vanadium source concentration made in ionized water is that 15~30mol/L obtains suspension A；
3) dodecyldimethylamine oxide that 0.002~0.02g is added in suspension A stirs evenly to obtain solution B；
4) carbon cloth that solution B and step 1) are handled well is fitted into autoclave, is subsequently placed in reaction baking oven and carries out Hydro-thermal reaction；
5) to which after reaction, reaction kettle is cooled to room temperature, after product deionized water and ethyl alcohol alternating flushing for several times Vacuum drying obtains the VS with hierarchical structure2Nano-chip arrays electrode material.
Step 1) the vacuum drying temperature is 40~60 DEG C, and drying time is 4~12h.
The vanadium source of the step 2) be vanadium acetylacetonate, sodium metavanadate or 12 hydration one of sodium vanadates or it is a kind of with The mixture of upper arbitrary proportion.
The sulphur source of the step 2) is one of thiocarbamide, thioacetamide and vulcanized sodium or more than one arbitrary proportions Mixture.
Step 4) the hydrothermal temperature is 150~170 DEG C, and the reaction time is 18~26h.
Step 5) the vacuum drying temperature is 40~60 DEG C, and drying time is 4~12h.
The present invention uses efficient, simple and inexpensive one step hydro thermal method, and vanadium disulfide nanometer sheet is prepared on carbon cloth Electrolysis water Hydrogen Evolution Performance is effectively promoted in array elctro-catalyst.
Compared with prior art, the present invention can obtain following the utility model has the advantages that
1) present invention is by introducing dodecyldimethylamine oxide as surfactant, using a step hydrothermal method, Pattern is made uniformly and there is the VS of hierarchical structure2Nano-chip arrays electrode material.
2) step water-heat process of the present invention, at low cost, reaction time is short, reaction condition is mild, preparation process is simple Single, stable product quality and pattern is uniform is environmentally friendly, can be suitble to be mass produced.
3) VS prepared by the present invention with hierarchical structure2Nano-chip arrays greatly improve the catalytic activity of catalyst, The nanometer chip architecture of two-dimensional ultrathin, exposes more active sites, can be used as the excellent electro-catalysis production oxygen electricity of one kind and urges Agent, in 100mA/cm2Current density under, overpotential can be down to 369mV.
Detailed description of the invention
Fig. 1 is the VS being grown on carbon cloth prepared by the embodiment of the present invention 32X-ray diffraction (XRD) map；
Fig. 2 is the VS being grown on carbon cloth prepared by the embodiment of the present invention 32Scanning electron microscope (SEM) photo；
Fig. 3 is the VS being grown on carbon cloth prepared by the embodiment of the present invention 32Linear sweep voltammetry (LSV) performance test Figure.
Specific embodiment
With reference to the accompanying drawing and specific embodiment the invention will be described in further detail:
Embodiment 1:
1) carbon cloth of (1 × 5) cm is handled using electrochemistry anodic oxidation, selected electrolyte is that concentration is 3mol/L ammonium dihydrogen phosphate, Faradaic current 0.2A, then in 40 DEG C of vacuum drying 12h；
2) vanadium acetylacetonate and thioacetamide are taken by the molar ratio of 1:3,25ml is added in vanadium source and sulphur source under stiring The vanadium source concentration made in deionized water is that 15mol/L obtains suspension A；
3) dodecyldimethylamine oxide that 0.002g is added in suspension A stirs evenly to obtain solution B；
4) carbon cloth that solution B and step 1) are handled well is fitted into autoclave, is subsequently placed in reaction baking oven 150 DEG C hydro-thermal reaction 18h；
5) to which after reaction, reaction kettle is cooled to room temperature, product deionized water and ethyl alcohol alternately rinse 3 times after 40 DEG C of vacuum drying 12h obtain the VS with hierarchical structure2Nano-chip arrays electrode material.
Embodiment 2:
1) carbon cloth of (1 × 5) cm is handled using electrochemistry anodic oxidation, selected electrolyte is that concentration is 4mol/L ammonium dihydrogen phosphate, Faradaic current 0.4A, then in 50 DEG C of vacuum drying 10h；
2) sodium metavanadate and thiocarbamide are taken by the molar ratio of 1:5,30ml deionized water is added in vanadium source and sulphur source under stiring In the vanadium source concentration that makes be that 25mol/L obtains suspension A；
3) dodecyldimethylamine oxide that 0.003g is added in suspension A stirs evenly to obtain solution B；
4) carbon cloth that solution B and step 1) are handled well is fitted into autoclave, is subsequently placed in reaction baking oven 170 DEG C hydro-thermal reaction 20h；
5) to which after reaction, reaction kettle is cooled to room temperature, product deionized water and ethyl alcohol alternately rinse 3 times after 50 DEG C of vacuum drying 10h obtain the VS with hierarchical structure2Nano-chip arrays electrode material.
Embodiment 3:
1) carbon cloth of (1 × 5) cm is handled using electrochemistry anodic oxidation, selected electrolyte is that concentration is 5mol/L ammonium dihydrogen phosphate, Faradaic current 0.6A, then in 60 DEG C of vacuum drying 4h；
2) 12 hydration sodium vanadates and thioacetamide are taken by the molar ratio of 1:6, vanadium source and sulphur source is added under stiring The vanadium source concentration made in 35ml deionized water is that 30mol/L obtains suspension A；
3) dodecyldimethylamine oxide that 0.02g is added in suspension A stirs evenly to obtain solution B；
4) carbon cloth that solution B and step 1) are handled well is fitted into autoclave, is subsequently placed in reaction baking oven 160 DEG C hydro-thermal reaction 26h；
5) to which after reaction, reaction kettle is cooled to room temperature, product deionized water and ethyl alcohol alternately rinse 3 times after 60 DEG C of vacuum drying 4h obtain the VS with hierarchical structure2Nano-chip arrays electrode material.
VS manufactured in the present embodiment2/ CC electrode material, the position that as can be seen from Figure 1 X-ray diffraction peak occurs indicate For VS2Characteristic peak, show successfully to synthesize VS2Electrode material.
It can be seen that the sample is the nano-chip arrays grown on carbon cloth from the SEM figure of Fig. 2, form with level The VS of structure2Nano-chip arrays electrode material.
It is 100mA/cm that the sample be can be seen that from the linear sweep voltammetry figure of Fig. 3 in current density2When, it has Low overpotential, down to 369mV, material has good electrocatalytic hydrogen evolution activity.
Embodiment 4:
1) carbon cloth of (1 × 5) cm is handled using electrochemistry anodic oxidation, selected electrolyte is that concentration is 3.5mol/L ammonium dihydrogen phosphate, Faradaic current 0.3A, then in 55 DEG C of vacuum drying 6h；
2) mixture and vulcanized sodium that vanadium acetylacetonate and sodium metavanadate are taken by the molar ratio of 1:4, under stiring by vanadium source It is that 20mol/L obtains suspension A that the vanadium source concentration made in 40ml deionized water is added with sulphur source；
3) dodecyldimethylamine oxide that 0.01g is added in suspension A stirs evenly to obtain solution B；
4) carbon cloth that solution B and step 1) are handled well is fitted into autoclave, is subsequently placed in reaction baking oven 155 DEG C hydro-thermal reaction is for 24 hours；
5) to which after reaction, reaction kettle is cooled to room temperature, product deionized water and ethyl alcohol alternately rinse 4 times after 55 DEG C of vacuum drying 6h obtain the VS with hierarchical structure2Nano-chip arrays electrode material.
Embodiment 5:
1) carbon cloth of (1 × 5) cm is handled using electrochemistry anodic oxidation, selected electrolyte is that concentration is 4.5mol/L ammonium dihydrogen phosphate, Faradaic current 0.5A, then in 45 DEG C of vacuum drying 8h；
2) vanadium acetylacetonate, the mixture of sodium metavanadate and 12 hydration sodium vanadates and thio second are taken by the molar ratio of 1:6 The mixture of amide and thiocarbamide, the vanadium source concentration made in 30ml deionized water, which is added, in vanadium source and sulphur source under stiring is 28mol/L obtains suspension A；
3) dodecyldimethylamine oxide that 0.015g is added in suspension A stirs evenly to obtain solution B；
4) carbon cloth that solution B and step 1) are handled well is fitted into autoclave, is subsequently placed in reaction baking oven 165 DEG C hydro-thermal reaction 20h；
5) to which after reaction, reaction kettle is cooled to room temperature, product deionized water and ethyl alcohol alternately rinse 5 times after 45 DEG C of vacuum drying 8h obtain the VS with hierarchical structure2Nano-chip arrays electrode material.

Claims (6)

1. a kind of VS with hierarchical structure2The synthetic method of nano-chip arrays electrode material, it is characterised in that:
1) carbon cloth is handled using electrochemistry anodic oxidation, selected electrolyte is that concentration is 3~5mol/L ammonium dihydrogen phosphate, electrolysis Electric current is 0.2~0.6A, is then dried in vacuo；
2) by 1:(3~6) molar ratio take vanadium source and sulphur source, 25ml-40ml deionization is added in vanadium source and sulphur source under stiring The vanadium source concentration made in water is that 15~30mol/L obtains suspension A；
3) dodecyldimethylamine oxide that 0.002~0.02g is added in suspension A stirs evenly to obtain solution B；
4) carbon cloth that solution B and step 1) are handled well is fitted into autoclave, is subsequently placed in reaction baking oven and carries out hydro-thermal Reaction；
5) to which after reaction, reaction kettle is cooled to room temperature, product deionized water and ethyl alcohol alternately rinse rear vacuum for several times It is dried to obtain the VS with hierarchical structure2Nano-chip arrays electrode material.
2. the VS according to claim 1 with hierarchical structure2The synthetic method of nano-chip arrays electrode material, feature Be: the step 1) vacuum drying temperature is 40~60 DEG C, and drying time is 4~12h.
3. the VS according to claim 1 with hierarchical structure2The synthetic method of nano-chip arrays electrode material, feature Be: the vanadium source of the step 2) be vanadium acetylacetonate, sodium metavanadate or 12 hydration one of sodium vanadates or more than one The mixture of arbitrary proportion.
4. the VS according to claim 1 with hierarchical structure2The synthetic method of nano-chip arrays electrode material, feature Be: the sulphur source of the step 2) is one of thiocarbamide, thioacetamide and vulcanized sodium or more than one arbitrary proportions Mixture.
5. the VS according to claim 1 with hierarchical structure2The synthetic method of nano-chip arrays electrode material, feature Be: the step 4) hydrothermal temperature is 150~170 DEG C, and the reaction time is 18~26h.
6. the VS according to claim 1 with hierarchical structure2The synthetic method of nano-chip arrays electrode material, feature Be: the step 5) vacuum drying temperature is 40~60 DEG C, and drying time is 4~12h.
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CN110064410A (en) * 2019-05-10 2019-07-30 深圳大学 A method of it is extremely easy to prepare the monatomic catalyst of noble metal
CN110064409A (en) * 2019-05-10 2019-07-30 深圳大学 A kind of Pt/VS2Catalysis material and its preparation method and application
CN110171828A (en) * 2019-06-14 2019-08-27 陕西科技大学 A kind of FeS nano material and its preparation method and application based on carbon cloth oriented growth
CN113206235A (en) * 2021-04-30 2021-08-03 陕西科技大学 Multi-component (V, Zn) metal sulfide and preparation method thereof
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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Cited By (11)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN110064410A (en) * 2019-05-10 2019-07-30 深圳大学 A method of it is extremely easy to prepare the monatomic catalyst of noble metal
CN110064409A (en) * 2019-05-10 2019-07-30 深圳大学 A kind of Pt/VS2Catalysis material and its preparation method and application
CN110064409B (en) * 2019-05-10 2022-03-11 深圳大学 Pt/VS2Catalytic material, preparation method and application thereof
CN110171828A (en) * 2019-06-14 2019-08-27 陕西科技大学 A kind of FeS nano material and its preparation method and application based on carbon cloth oriented growth
CN110171828B (en) * 2019-06-14 2021-02-09 陕西科技大学 FeS nano material based on carbon cloth directional growth and preparation method and application thereof
CN113206235A (en) * 2021-04-30 2021-08-03 陕西科技大学 Multi-component (V, Zn) metal sulfide and preparation method thereof
CN113206235B (en) * 2021-04-30 2022-11-18 陕西科技大学 Multi-component (V, zn) metal sulfide and preparation method thereof
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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