CN109772366A - A kind of preparation method of cuprous sulfide/vanadium trioxide as full PH elctro-catalyst - Google Patents
A kind of preparation method of cuprous sulfide/vanadium trioxide as full PH elctro-catalyst Download PDFInfo
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- CN109772366A CN109772366A CN201910202640.3A CN201910202640A CN109772366A CN 109772366 A CN109772366 A CN 109772366A CN 201910202640 A CN201910202640 A CN 201910202640A CN 109772366 A CN109772366 A CN 109772366A
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- elctro
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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
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Abstract
A kind of preparation method of cuprous sulfide/vanadium trioxide as full PH elctro-catalyst, foam copper is successively immersed in pure acetone solution and hydrochloric acid solution and is cleaned by ultrasonic, and then replaces with deionized water the foam copper that obtains that treated of vacuum drying after flushing with ethyl alcohol respectively；Sodium metavanadate, thioacetamide are dissolved in deionized water and obtain suspension A；The foam copper that suspension A and step 1) are handled well, it is fitted into autoclave, it is subsequently placed in reaction baking oven and cools down reaction kettle at room temperature after hydro-thermal reaction, product uses deionized water and ethyl alcohol flushing, and vacuum drying obtains cuprous sulfide/vanadium trioxide as full PH elctro-catalyst afterwards several times.For the present invention using sodium metavanadate as vanadium source, thioacetamide is sulphur source, through one step hydro thermal method on foam copper success fabricated in situ Cu2S/V2O3.Its is at low cost, reaction time is short, and reaction condition is mild, preparation process is simple, stable product quality and pattern is uniform, environmentally friendly, can be suitble to be mass produced.
Description
Technical field
The invention belongs to electrolysis water catalytic fields, are related to a kind of preparation method of electrolysis water catalytic electrode material, specifically relate to
And a kind of preparation method of cuprous sulfide/vanadium trioxide as full PH elctro-catalyst.
Background technique
Cu2S is a kind of important p-type semiconductor material, in solar battery, thermocouple, photovoltaic device and lithium ion battery
Etc. be widely used.The Cu of nanostructure2S due to special physics and chemical property, make its catalysis, mechanics,
The fields such as calorifics, electricity, optics have significant application value, to obtain the pay attention to day by day of researcher.In recent years, no
With the Cu of pattern2S nano crystal material, such as cuprous sulfide nanosphere, cuprous sulfide nanometer sheet, cuprous sulfide nano flower, sulphur
Change cuprous nanometer rods etc. to be synthesized.Wherein, three-dimensional (3D) the structure nano microballoon being self-assembly of by nanometer sheet, has
Biggish specific surface area, stronger adsorption energy and faster photoelectricity transmission performance make it have important Research Prospects.In addition, will
Catalyst can be effectively facilitated charge transmission in conjunction with conductive substrates, and can significantly enhance its catalytic activity and stabilization
Property.
Summary of the invention
The purpose of the present invention is to provide a kind of preparation processes simply, reaction is mild and low-cost cuprous sulfide/tri-
Preparation method of the V 2 O as full PH elctro-catalyst, the Cu according to said method prepared2S/V2O3Purity is high, morphology and size are equal
One, 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) foam copper is successively immersed in pure acetone solution and hydrochloric acid solution and is cleaned by ultrasonic, then respectively with ethyl alcohol and go from
The vacuum drying foam copper that obtains that treated after sub- water alternately rinses；
2) be 1:(3~6 by vanadium source and sulphur source) molar ratio sodium metavanadate, thioacetamide are dissolved in 25-35ml's
In deionized water, the suspension A that vanadium source concentration is 15~30mmol/L is obtained；
3) foam copper for handling suspension A and step 1) well is fitted into autoclave, is subsequently placed in reaction baking oven
In at 140~180 DEG C, 18~26h of hydro-thermal reaction；
4) to which after reaction, reaction kettle is cooled down at room temperature, after product deionized water and ethyl alcohol flushing several times
Vacuum drying obtains cuprous sulfide/vanadium trioxide as full PH elctro-catalyst.
The size of the foam copper of the step 1) is 2 × 4cm.
The concentration of the hydrochloric acid solution of the step 1) is 2~4mol/L.
The ultrasonic cleaning time of the step 1) is 5~10min.
The ethyl alcohol of the step 1) replaces flushing 3~5 times with deionized water.
The vacuum drying temperature of the step 1) is 40~60 DEG C, and drying time is 4~10h.
The vacuum drying temperature of the step 4) is 40~60 DEG C, and drying time is 6~14h.
For the present invention using sodium metavanadate as vanadium source, thioacetamide is sulphur source, and through one step hydro thermal method, success is former on foam copper
Position synthesis Cu2S/V2O3。
Compared with prior art, the invention has the following advantages:
(1) present invention chooses suitable sulphur source and vanadium source and Cu of uniform morphology is made using a step hydrothermal method2S/
V2O3。
(2) present invention uses a step water-heat process, and 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) Cu that nanometer sheet prepared by the present invention is self-assembly of2S/V2O3Nanosphere greatly improves catalyst
Catalytic activity, three-dimensional multistage nanometer chip architecture expose more active sites, can be used as a kind of excellent elctro-catalyst,
In 100mA/cm2Current density under, the overpotential in acid, alkalinity and neutrality is respectively can be down to 405,390,415mV.
Detailed description of the invention
Fig. 1 is Cu of the growth in situ of the preparation of the embodiment of the present invention 2 on foam copper2S/V2O3X-ray diffraction (XRD)
Map；
Fig. 2 is Cu of the growth in situ of the preparation of the embodiment of the present invention 2 on foam copper2S/V2O3Scanning electron microscope (SEM) shine
Piece；
Fig. 3 is Cu of the growth in situ of the preparation of the embodiment of the present invention 2 on foam copper2S/V2O3Linear 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) foam copper of 2 × 4cm is immersed in pure acetone solution and is cleaned by ultrasonic 5min, then immerse the hydrochloric acid of 2mol/L again
It is cleaned by ultrasonic 5min in solution, then replaces flushing 3 times with deionized water with ethyl alcohol respectively, finally obtained in 60 DEG C of vacuum drying 4h
To treated foam copper；
2) sodium metavanadate, thioacetamide are dissolved in the deionized water of 25ml by the molar ratio for being 1:3 by vanadium source and sulphur source
In, obtain the suspension A that vanadium source concentration is 15mmol/L；
3) foam copper for handling suspension A and step 1) well is fitted into autoclave, is subsequently placed in reaction baking oven
In at 140 DEG C, hydro-thermal reaction 26h；
4) to which after reaction, reaction kettle is cooled down at room temperature, product deionized water and ethyl alcohol rinse 5 times after 60
DEG C vacuum drying 6h obtain cuprous sulfide/vanadium trioxide as full PH elctro-catalyst.
Embodiment 2:
1) foam copper of 2 × 4cm is immersed in pure acetone solution and is cleaned by ultrasonic 10min, then immerse the salt of 3mol/L again
It is cleaned by ultrasonic 10min in acid solution, then replaces flushing 4 times with deionized water with ethyl alcohol respectively, is finally dried in vacuo at 50 DEG C
6h obtains that treated foam copper；
2) sodium metavanadate, thioacetamide are dissolved in the deionized water of 30ml by the molar ratio for being 1:5 by vanadium source and sulphur source
In, obtain the suspension A that vanadium source concentration is 25mmol/L；
3) foam copper for handling suspension A and step 1) well is fitted into autoclave, is subsequently placed in reaction baking oven
In at 160 DEG C, hydro-thermal reaction is for 24 hours；
4) to which after reaction, reaction kettle is cooled down at room temperature, product deionized water and ethyl alcohol rinse 4 times after 50
DEG C vacuum drying 8h obtain cuprous sulfide/vanadium trioxide as full PH elctro-catalyst.
Cu manufactured in the present embodiment2S/V2O3Electrode material, the position table that as can be seen from Figure 1 X-ray diffraction peak occurs
It is shown as Cu2S/V2O3Characteristic peak, show successfully to synthesize Cu2S/V2O3Electrode material.
It can be seen that the sample is the Cu that nanometer sheet is self-assembly of from the SEM figure of Fig. 22S/V2O3Nanosphere.
It is 100mA/cm that the sample be can be seen that from the linear sweep voltammetry figure of Fig. 3 in current density2When, acid, alkali
Property and neutrality in overpotential be respectively 405,390,415mV, material has good electrocatalytic hydrogen evolution activity.
Embodiment 3:
1) foam copper of 2 × 4cm is immersed in pure acetone solution and is cleaned by ultrasonic 10min, then immerse the salt of 4mol/L again
It is cleaned by ultrasonic 10min in acid solution, then replaces flushing 5 times with deionized water with ethyl alcohol respectively, is finally dried in vacuo at 40 DEG C
10h obtains that treated foam copper；
2) sodium metavanadate, thioacetamide are dissolved in the deionized water of 35ml by the molar ratio for being 1:6 by vanadium source and sulphur source
In, obtain the suspension A that vanadium source concentration is 30mmol/L；
3) foam copper for handling suspension A and step 1) well is fitted into autoclave, is subsequently placed in reaction baking oven
In at 180 DEG C, hydro-thermal reaction 18h；
4) to which after reaction, reaction kettle is cooled down at room temperature, product deionized water and ethyl alcohol rinse 4 times after 40
DEG C vacuum drying 14h obtain cuprous sulfide/vanadium trioxide as full PH elctro-catalyst.
Embodiment 4:
1) foam copper of 2 × 4cm is immersed in pure acetone solution and is cleaned by ultrasonic 8min, then immerse the hydrochloric acid of 3mol/L again
It is cleaned by ultrasonic 6min in solution, then replaces flushing 5 times with deionized water with ethyl alcohol respectively, finally obtained in 45 DEG C of vacuum drying 8h
To treated foam copper；
2) sodium metavanadate, thioacetamide are dissolved in the deionized water of 28ml by the molar ratio for being 1:4 by vanadium source and sulphur source
In, obtain the suspension A that vanadium source concentration is 20mmol/L；
3) foam copper for handling suspension A and step 1) well is fitted into autoclave, is subsequently placed in reaction baking oven
In at 150 DEG C, hydro-thermal reaction 25h；
4) to which after reaction, reaction kettle is cooled down at room temperature, product deionized water and ethyl alcohol rinse 3 times after 55
DEG C vacuum drying 10h obtain cuprous sulfide/vanadium trioxide as full PH elctro-catalyst.
Embodiment 5:
1) foam copper of 2 × 4cm is immersed in pure acetone solution and is cleaned by ultrasonic 6min, then immerse the hydrochloric acid of 4mol/L again
It is cleaned by ultrasonic 8min in solution, then replaces flushing 4 times with deionized water with ethyl alcohol respectively, finally obtained in 55 DEG C of vacuum drying 5h
To treated foam copper；
2) sodium metavanadate, thioacetamide are dissolved in the deionized water of 32ml by the molar ratio for being 1:5 by vanadium source and sulphur source
In, obtain the suspension A that vanadium source concentration is 28mmol/L；
3) foam copper for handling suspension A and step 1) well is fitted into autoclave, is subsequently placed in reaction baking oven
In at 170 DEG C, hydro-thermal reaction 20h；
4) to which after reaction, reaction kettle is cooled down at room temperature, product deionized water and ethyl alcohol rinse 5 times after 45
DEG C vacuum drying 12h obtain cuprous sulfide/vanadium trioxide as full PH elctro-catalyst.
Claims (7)
1. a kind of preparation method of cuprous sulfide/vanadium trioxide as full PH elctro-catalyst, it is characterised in that including following step
It is rapid:
1) foam copper is successively immersed in pure acetone solution and hydrochloric acid solution and is cleaned by ultrasonic, then use ethyl alcohol and deionized water respectively
The vacuum drying foam copper that obtains that treated after alternately rinsing；
2) be 1:(3~6 by vanadium source and sulphur source) molar ratio by sodium metavanadate, thioacetamide be dissolved in 25-35ml go from
In sub- water, the suspension A that vanadium source concentration is 15~30mmol/L is obtained；
3) foam copper for handling suspension A and step 1) well is fitted into autoclave, is subsequently placed in reaction baking oven
140~180 DEG C, 18~26h of hydro-thermal reaction；
4) to which after reaction, reaction kettle is cooled down at room temperature, product deionized water and ethyl alcohol rinse rear vacuum several times
Cuprous sulfide/vanadium trioxide is dried to obtain as full PH elctro-catalyst.
2. preparation method of the cuprous sulfide/vanadium trioxide according to claim 1 as full PH elctro-catalyst, feature
Be: the size of the foam copper of the step 1) is 2 × 4cm.
3. preparation method of the cuprous sulfide/vanadium trioxide according to claim 1 as full PH elctro-catalyst, feature
Be: the concentration of the hydrochloric acid solution of the step 1) is 2~4mol/L.
4. preparation method of the cuprous sulfide/vanadium trioxide according to claim 1 as full PH elctro-catalyst, feature
Be: the ultrasonic cleaning time of the step 1) is 5~10min.
5. preparation method of the cuprous sulfide/vanadium trioxide according to claim 1 as full PH elctro-catalyst, feature
Be: the ethyl alcohol of the step 1) replaces flushing 3~5 times with deionized water.
6. preparation method of the cuprous sulfide/vanadium trioxide according to claim 1 as full PH elctro-catalyst, feature
Be: the vacuum drying temperature of the step 1) is 40~60 DEG C, and drying time is 4~10h.
7. preparation method of the cuprous sulfide/vanadium trioxide according to claim 1 as full PH elctro-catalyst, feature
Be: the vacuum drying temperature of the step 4) is 40~60 DEG C, and drying time is 6~14h.
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Cited By (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN110581284A (en) * | 2019-09-30 | 2019-12-17 | 陕西科技大学 | Electrocatalysis function V2O3Preparation method and application of @ Co |
| CN110699701A (en) * | 2019-09-06 | 2020-01-17 | 华东理工大学 | Foam nickel loaded with metal nickel and vanadium trioxide compound and preparation method and application thereof |
| CN110711590A (en) * | 2019-10-10 | 2020-01-21 | 安徽师范大学 | One-dimensional cobalt-sulfur compound/cuprous sulfide compound nano-array @ foamy copper material and preparation method and application thereof |
| CN112811467A (en) * | 2021-01-18 | 2021-05-18 | 陕西科技大学 | V-shaped groove2O3Method for preparing nanoparticles |
| CN113184906A (en) * | 2021-05-13 | 2021-07-30 | 陕西科技大学 | One-step hydrothermal method for preparing V2O3Method of nanosphere |
| CN113213543A (en) * | 2021-05-13 | 2021-08-06 | 陕西科技大学 | MnO (MnO)2/V2O3Process for preparing nano composite material |
| CN113652711A (en) * | 2021-09-13 | 2021-11-16 | 陕西科技大学 | V-FeS/IF electro-catalytic material and preparation method thereof |
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Cited By (9)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN110699701A (en) * | 2019-09-06 | 2020-01-17 | 华东理工大学 | Foam nickel loaded with metal nickel and vanadium trioxide compound and preparation method and application thereof |
| CN110581284A (en) * | 2019-09-30 | 2019-12-17 | 陕西科技大学 | Electrocatalysis function V2O3Preparation method and application of @ Co |
| CN110581284B (en) * | 2019-09-30 | 2020-12-08 | 陕西科技大学 | Electrocatalysis function V2O3Preparation method and application of @ Co |
| CN110711590A (en) * | 2019-10-10 | 2020-01-21 | 安徽师范大学 | One-dimensional cobalt-sulfur compound/cuprous sulfide compound nano-array @ foamy copper material and preparation method and application thereof |
| CN110711590B (en) * | 2019-10-10 | 2022-11-22 | 安徽师范大学 | One-dimensional cobalt-sulfur compound/cuprous sulfide compound nano-array @ foamy copper material and preparation method and application thereof |
| CN112811467A (en) * | 2021-01-18 | 2021-05-18 | 陕西科技大学 | V-shaped groove2O3Method for preparing nanoparticles |
| CN113184906A (en) * | 2021-05-13 | 2021-07-30 | 陕西科技大学 | One-step hydrothermal method for preparing V2O3Method of nanosphere |
| CN113213543A (en) * | 2021-05-13 | 2021-08-06 | 陕西科技大学 | MnO (MnO)2/V2O3Process for preparing nano composite material |
| CN113652711A (en) * | 2021-09-13 | 2021-11-16 | 陕西科技大学 | V-FeS/IF electro-catalytic material and preparation method thereof |
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