CN108315759A - A kind of Cu of vanadium modification2S self-supportings electrode material and its synthetic method - Google Patents
A kind of Cu of vanadium modification2S self-supportings electrode material and its synthetic method Download PDFInfo
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- CN108315759A CN108315759A CN201810212306.1A CN201810212306A CN108315759A CN 108315759 A CN108315759 A CN 108315759A CN 201810212306 A CN201810212306 A CN 201810212306A CN 108315759 A CN108315759 A CN 108315759A
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- C25—ELECTROLYTIC OR ELECTROPHORETIC PROCESSES; APPARATUS THEREFOR
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- C25B1/00—Electrolytic production of inorganic compounds or non-metals
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Abstract
The present invention provides a kind of Cu of vanadium modification2The synthetic method of S self-supporting electrode materials, includes the following steps：It is 1 that clean foam copper, which is immersed a concentration of 10 ~ 40 mM in vanadium source, vanadium source and sulphur source molar ratio,:（1~10）Suspension in, carry out solvent thermal reaction, fully reaction after, obtain V modification Cu2S self-supporting electrode materials.The Cu of the V modifications prepared by this method is also disclosed in the present invention2S self-supporting electrode materials.This method directly synthesizes final product using a step solvent thermal reaction, has low synthesis temperature, and easy to operate and reaction is mild, 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 mass produce.
Description
Technical field
The invention belongs to electrode material surface processing technology fields, and in particular to a kind of Cu of vanadium modification2S self-supporting electrode materials
The synthetic method of material.
Background technology
Nowadays, with the rapid development of economy, energy problem and problem of environmental pollution getting worse, and finding cleaning can
Continuous energy is the breach for solving this two hang-up, and Hydrogen Energy expresses it as green sustainable energy of new generation, people
Great expectations.Water-splitting technology is to realize sustainable one of the effective way for preparing hydrogen, however, current common water-splitting catalyst
It is still based on the material of precious metals pt, this severely limits the scale of water-splitting, industrialization.To solve this problem,
People are sought for substituting Pt sills based on the high transition metal based compound of earth's crust reserves.In recent years, to base metal
The exploration of catalyst achieves greater advance, but is largely focused on the transition metal elements such as molybdenum, tungsten, nickel, cobalt.Although elemental copper
It is abundant with crustal abundance height, biological relevance, chemical valence state（Cu0, CuI, CuIIAnd CuIII）With abundant chemical coordination
The features such as, however the research for producing hydrogen catalyst as electro-catalysis water-splitting based on the compound of copper is but relatively seldom.
Chinese invention issued patents the 201610343133.8th disclose a kind of noble metal nanocrystalline loaded Cu SbS2It receives
The composite material of the preparation method of meter Jing, gained has excellent photocatalysis performance, can be used for photoelectrocatalysis field, but operates
Step is complicated, and reaction time is longer, and technical difficulty is big.Chinese invention issued patents the 201610163670.4th disclose one
Kind different-shape self assembly Cu2The preparation of S nano materials is first reacted 2 ~ 6 hours under nitrogen protection, then forged under an inert gas
Burning obtains different-shape self assembly Cu2S nano materials, preparation process is complicated, and reaction time is long, severe reaction conditions, and cost
Greatly.
Therefore, the Cu that a kind of preparation process is simple, reaction condition is mild, environmental-friendly is explored2The preparation method of S material at
It is an urgent problem to be solved currently.
Invention content
This patent is directed to the deficiency of above-mentioned material, proposes a kind of Cu of vanadium modification2The synthesis side of S self-supporting electrode materials
Method, this method is easy to operate, and reaction condition is mild, and reaction time is short, is suitble to large-scale application.The material can be used as a kind of excellent
Electrocatalytic hydrogen evolution elctro-catalyst.To achieve the goals above, the present invention uses following technical scheme.
To achieve the goals above, the technical solution adopted in the present invention is：A kind of Cu of vanadium modification2S self-supporting electrodes
The synthetic method of material, includes the following steps：
（1）Foam copper is immersed in successively in acetone, hydrochloric acid and water and ethyl alcohol and is cleaned by ultrasonic, is then dried in vacuo, hydrochloric acid is dense
Degree is 1 ~ 5 mol/L；
（2）It is raw material to select 12 hydration sodium vanadates and thioacetamide, weighs certain mass, control vanadium source and sulphur source molar ratio
It is 1:（1~10）, be dissolved in suitable solvent so that a concentration of 10 ~ 40 mM in vanadium source, stir 3 ~ 20 min, obtain suspended
Liquid A；
（3）The suspension A being stirred is poured into the water heating kettle of 50 mL polytetrafluoroethyllining linings, by step（1）Pretreated bubble
Sealing after foam copper is put into polytetrafluoroethyllining lining, is subsequently placed in homogeneous reaction instrument and reacts；
（4）After reaction, reaction kettle is cooled down at room temperature, product deionized water and ethyl alcohol alternately rinse for several times, vacuum
It is dry, obtain the Cu of vanadium modification2S self-supporting electrode materials.
Step（1）The ultrasonic cleaning is 5 ~ 15 min.
Step（1）The vacuum drying is 5 ~ 15 h of vacuum drying at 20 ~ 40 DEG C.
Step（2）The solvent is one or more of deionized water, absolute ethyl alcohol, methanol, ethylene glycol.
Step（3）The solvent thermal reaction temperature is 70 ~ 200 DEG C, and the reaction time is 1 ~ 30 h.
Step（4）The vacuum drying is 3 ~ 15 h of vacuum drying at 20 ~ 40 DEG C.
Compared with prior art, the present invention can obtain following advantageous effect：
（1）This method directly synthesizes final product using a step solvent thermal reaction, has low synthesis temperature, easy to operate
And reaction is mild, 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 extensive
Production.
（2）The Cu of vanadium modification prepared by this method2S self-supporting electrode materials, pattern is uniform, and purity is high.Meanwhile foam copper
The unique three-dimensional porous structure of substrate, improves the transmittability of charge.Then its chemical property can be greatly enhanced.
（3）Vanadium and Cu2The synergistic effect that S is generated, improves the active site of material, as electrolysis aquatic products hydrogen electrode
Excellent chemical property can be shown when material, in 10 mA/cm2Current density under, overpotential is about 280 mV,
In 100 mA/cm2Current density under, overpotential is about 470 mV, and material is with good stability.
Description of the drawings
Fig. 1 is the Cu of vanadium modification prepared by the embodiment of the present invention 32The X-ray diffraction of S self-supporting electrode materials（XRD）Figure
Spectrum；
Fig. 2 is the Cu of vanadium modification prepared by the embodiment of the present invention 32The scanning electron microscope of S self-supporting electrode materials（SEM）Photo；
Fig. 3 is the Cu of vanadium modification prepared by the embodiment of the present invention 32The linear sweep voltammetry of S self-supporting electrode materials（LSV）Performance
Test chart.
Specific implementation mode
Below in conjunction with the accompanying drawings and specific embodiment is described in further detail the present invention, but the present invention is not limited to
Following embodiment.
Embodiment 1：
（1）It will（2×5）The foam copper of cm be immersed in be cleaned by ultrasonic 5 min in acetone, be immersed in again in the hydrochloric acid of 1 mol/L into
Row is cleaned by ultrasonic 5 min, finally replaces flushing 3 times with deionized water with ethyl alcohol respectively, is obtained after 5 h are dried in vacuo at 20 DEG C
To treated foam copper；
（2）It is raw material to choose 12 hydration sodium vanadates and thioacetamide, and it is 0.2mmol to take 12 hydration sodium vanadates, controls vanadium
The molar ratio of source and sulphur source is 1：1, while being added in 20 ml absolute ethyl alcohols, 3 min of magnetic agitation is obtained suspended at room temperature
Liquid A；
（3）The suspension A and step that will be stirred（1）Pretreated foam copper is put into close in 50 mL polytetrafluoroethyllining linings
Envelope, is subsequently placed in homogeneous reaction instrument and reacts, and the reaction time is to be reacted under 1 h condition at 70 DEG C；
（4）After reaction terminates, cools down, product deionized water and ethyl alcohol alternately rinse 3 times, are then dried in vacuo 5 at 20 DEG C
H obtains a kind of Cu of vanadium modification2S self-supporting electrode materials.
Embodiment 2：
（1）It will（2×5）The foam copper of cm be immersed in be cleaned by ultrasonic 5 min in acetone, be immersed in again in the hydrochloric acid of 2 mol/L into
Row is cleaned by ultrasonic 5 min, finally replaces flushing 3 times with deionized water with ethyl alcohol respectively, is obtained after 10 h are dried in vacuo at 20 DEG C
To treated foam copper；
（2）It is raw material to choose 12 hydration sodium vanadates and thioacetamide, and it is 0.4mmol to take 12 hydration sodium vanadates, controls vanadium
The molar ratio of source and sulphur source is 1：1, while being added in the mixed liquor of 25 ml absolute ethyl alcohols and water, magnetic agitation 5 at room temperature
Min obtains suspension A；
（3）The suspension A and step that will be stirred（1）Pretreated foam copper is put into close in 50 mL polytetrafluoroethyllining linings
Envelope, is subsequently placed in homogeneous reaction instrument and reacts, and the reaction time is to be reacted under 5 h conditions at 100 DEG C；
（4）After reaction terminates, cools down, product deionized water and ethyl alcohol alternately rinse 3 times, are then dried in vacuo at 20 DEG C
10 h obtain the Cu of vanadium modification2S self-supporting electrode materials.
Embodiment 3：
（1）It will（2×5）The foam copper of cm, which is immersed in, to be cleaned by ultrasonic 5 min, is immersed in the hydrochloric acid of 3mol/L and carries out again in acetone
It is cleaned by ultrasonic 10 min, finally replaces flushing 3 times with deionized water with ethyl alcohol respectively, obtained after 5 h are dried in vacuo at 30 DEG C
Treated foam copper；
（2）It is raw material to choose 12 hydration sodium vanadates and thioacetamide, and it is 0.8 mmol to take 12 hydration sodium vanadates, controls vanadium
The molar ratio of source and sulphur source is 1：2, while being added in 30 ml methanol, 10 min of magnetic agitation obtains suspension at room temperature
A；
（3）The suspension A and step that will be stirred（1）Pretreated foam copper is put into close in 50 mL polytetrafluoroethyllining linings
Envelope, is subsequently placed in homogeneous reaction instrument and reacts, and the reaction time is to be reacted under 10 h conditions at 120 DEG C；
（4）After reaction terminates, cools down, product deionized water and ethyl alcohol alternately rinse 3 times, are then dried in vacuo 5 at 30 DEG C
H obtains the Cu of vanadium modification2S self-supporting electrode materials.
The Cu of vanadium modification manufactured in the present embodiment2S self-supporting electrode materials, as can be seen from Figure 1 X-ray powder diffraction
The position that peak occurs is expressed as the Cu of two kinds of phases2S, no other mutually generate, and show that vanadium is present in the form of adulterating in material.
From the SEM it can be seen from the figure thats of Fig. 2, the sample is in spherical distribution, and pattern is uniform.
From the linear sweep voltammetry it can be seen from the figure that of Fig. 3, which is 10 mA/cm in current density2When, it has
Overpotential low 280 mV, in 100 mA/cm2Current density under, overpotential is 470 mV, and it is good to show that the material has
Electrocatalytic hydrogen evolution activity.
Embodiment 4：
（1）It will（2×5）The foam copper of cm be immersed in be cleaned by ultrasonic 5 min in acetone, be immersed in again in the hydrochloric acid of 3 mol/L into
Row is cleaned by ultrasonic 13 min, finally replaces flushing 3 times with deionized water with ethyl alcohol respectively, after 10 h are dried in vacuo at 30 DEG C
The foam copper that obtains that treated；
（2）It is raw material to choose 12 hydration sodium vanadates and thioacetamide, and it is 1.2 mmol to take 12 hydration sodium vanadates, controls vanadium
The molar ratio of source and sulphur source is 1：6, while being added in 30 ml absolute ethyl alcohols, 15 min of magnetic agitation is hanged at room temperature
Turbid A；
（3）The suspension A and step that will be stirred（1）Pretreated foam copper is put into close in 50 mL polytetrafluoroethyllining linings
Envelope, is subsequently placed in homogeneous reaction instrument and reacts, and the reaction time is to be reacted under 15 h conditions at 160 DEG C；
（4）After reaction terminates, cools down, product deionized water and ethyl alcohol alternately rinse 3 times, are then dried in vacuo at 30 DEG C
10 h obtain the Cu of vanadium modification2S self-supporting electrode materials.
Embodiment 5：
（1）It will（2×5）The foam copper of cm be immersed in be cleaned by ultrasonic 5 min in acetone, be immersed in again in the hydrochloric acid of 5 mol/L into
Row is cleaned by ultrasonic 15 min, finally replaces flushing 3 times with deionized water with ethyl alcohol respectively, after 15 h are dried in vacuo at 40 DEG C
The foam copper that obtains that treated；
（2）It is raw material to choose 12 hydration sodium vanadates and thioacetamide, and it is 0.5 mmol to take 12 hydration sodium vanadates, controls vanadium
The molar ratio of source and sulphur source is 1：10, while being added in 40 ml ethylene glycol, 20 min of magnetic agitation is obtained suspended at room temperature
Liquid A；
（3）The suspension A and step that will be stirred（1）Pretreated foam copper is put into close in 50 mL polytetrafluoroethyllining linings
Envelope, is subsequently placed in homogeneous reaction instrument and reacts, and the reaction time is to be reacted under 30 h conditions at 200 DEG C；
（4）After reaction terminates, cools down, product deionized water and ethyl alcohol alternately rinse 3 times, are then dried in vacuo at 40 DEG C
15 h obtain the Cu of vanadium modification2S self-supporting electrode materials.
Claims (10)
1. a kind of Cu of vanadium modification2The synthetic method of S self-supporting electrode materials, which is characterized in that include the following steps：
It is 1 that clean foam copper, which is immersed a concentration of 10 ~ 40 mM in vanadium source, vanadium source and sulphur source molar ratio,:（1~10）Suspension
In, it carries out solvent thermal reaction and obtains the Cu of vanadium modification fully after reaction2S self-supporting electrode materials.
2. a kind of Cu of vanadium modification according to claim 12The synthetic method of S self-supporting electrode materials, which is characterized in that
The vanadium source includes 12 hydration sodium vanadates；The sulphur source includes thioacetamide.
3. a kind of Cu of vanadium modification according to claim 12The synthetic method of S self-supporting electrode materials, which is characterized in that
The solvent of the suspension is one or more in deionized water, absolute ethyl alcohol, methanol, ethylene glycol.
4. a kind of Cu of vanadium modification according to claim 12The synthetic method of S self-supporting electrode materials, which is characterized in that
The solvent thermal reaction temperature is 70 ~ 200 DEG C, and the reaction time is 1 ~ 30 h.
5. a kind of Cu of vanadium modification according to claim 12The synthetic method of S self-supporting electrode materials, which is characterized in that
Foam copper is pre-processed, foam copper is immersed in successively in acetone, hydrochloric acid and water and ethyl alcohol and is cleaned by ultrasonic, it is dry, it obtains clean
Net foam copper.
6. a kind of Cu of vanadium modification according to claim 12The synthetic method of S self-supporting electrode materials, which is characterized in that
After reaction, wait for that reaction system is down to room temperature, wash products are dry, obtain the Cu of clean vanadium modification2S self-supporting electrodes
Material.
7. according to a kind of Cu of vanadium modification of claim 1 ~ 6 any one of them2The synthetic method of S self-supporting electrode materials, it is special
Sign is that specific steps include：
1）Foam copper is immersed in successively in acetone, hydrochloric acid and water and ethyl alcohol and is cleaned by ultrasonic, is then dried in vacuo, concentration of hydrochloric acid
For 1 ~ 5 mol/L；
2）It is raw material to select 12 hydration sodium vanadates and thioacetamide, weighs certain mass, control vanadium source and sulphur source molar ratio
It is 1:（1~10）, be dissolved in suitable solvent so that a concentration of 10 ~ 40 mM in vanadium source, stir 3 ~ 20 min, obtain suspended
Liquid A；
3）The suspension A being stirred is poured into the water heating kettle of 50 mL polytetrafluoroethyllining linings, by step 1）Pretreated foam
Sealing after copper is put into polytetrafluoroethyllining lining, is subsequently placed in homogeneous reaction instrument and reacts；
4）After reaction, reaction kettle is cooled down at room temperature, product deionized water and ethyl alcohol alternately rinse for several times, and vacuum is dry
It is dry, obtain the Cu of vanadium modification2S self-supporting electrode materials.
8. a kind of Cu of vanadium modification according to claim 62The synthetic method of S self-supporting electrode materials, which is characterized in that
Step 1）The ultrasonic cleaning is 5 ~ 15 min.
9. a kind of Cu of vanadium modification according to claim 62The synthetic method of S self-supporting electrode materials, which is characterized in that
Step 1）The vacuum drying is 5 ~ 15 h of vacuum drying at 20 ~ 40 DEG C；Step 4）The vacuum drying is 20 ~ 40 DEG C
3 ~ 15 h of lower vacuum drying.
10. the Cu for the vanadium modification that any one of claim 1 ~ 9 obtains2S self-supporting electrode materials.
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Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN108866562A (en) * | 2018-06-29 | 2018-11-23 | 新奥科技发展有限公司 | Preparation method, self-supporting electrode material and the electrolysis unit of self-supporting electrode material |
| CN109261168A (en) * | 2018-10-16 | 2019-01-25 | 陕西科技大学 | A kind of Ni of vanadium modification3S2Nano-bar array electrode material and preparation method thereof |
| 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 |
| 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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| Publication number | Priority date | Publication date | Assignee | Title |
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| 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 |
| 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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