CN108315759B - A kind of Cu of vanadium modification2S self-supporting electrode material and its synthetic method - Google Patents
A kind of Cu of vanadium modification2S self-supporting electrode material and its synthetic method Download PDFInfo
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- CN108315759B CN108315759B CN201810212306.1A CN201810212306A CN108315759B CN 108315759 B CN108315759 B CN 108315759B CN 201810212306 A CN201810212306 A CN 201810212306A CN 108315759 B CN108315759 B CN 108315759B
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Abstract
The present invention provides a kind of Cu of vanadium modification2The synthetic method of S self-supporting electrode material, comprising the following steps: clean foam copper immerses to vanadium source concentration be 10 ~ 40 mM, vanadium source and sulphur source molar ratio be 1:(1 ~ 10) suspension in, carry out solvent thermal reaction, after sufficiently reacting, obtain the Cu that V is modified2S self-supporting electrode material.The Cu of the V modification prepared by this method is also disclosed in the present invention2S self-supporting electrode material.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, and at low cost, yield is high, is not necessarily to post-processing, environmentally friendly, can be suitble to be mass produced.
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 material
The synthetic method of material.
Background technique
Nowadays, with the rapid development of economy, energy problem and environmental pollution is getting worse, and finding cleaning can hold
The continuous energy is the breach for solving this two hang-up, and Hydrogen Energy expresses thickness to it as green sustainable energy of new generation, people
It hopes.Water-splitting technology is to realize sustainable one of the effective way for preparing hydrogen, however, current common water-splitting catalyst is still
It is so the material based on precious metals pt, this severely limits the scales of water-splitting, industrialization.To solve this problem, people
Be sought for substituting Pt sill based on the high transition metal based compound of earth's crust reserves.In recent years, base metal is urged
The exploration of agent achieves greater advance, but is largely focused on the transition metal elements such as molybdenum, tungsten, nickel, cobalt.Although elemental copper has
There are crustal abundance height, biological relevance, chemical valence state to enrich (Cu0, CuI, CuIIAnd CuIII) and chemical coordination abundant etc.
Feature, however it is but relatively seldom based on the research that the compound of copper produces hydrogen catalyst as electro-catalysis water-splitting.
Chinese invention issued patents the 201610343133.8th discloses a kind of noble metal nanocrystalline loaded Cu SbS2It receives
The preparation method of meter Jing, resulting composite material have excellent photocatalysis performance, can be used for photoelectrocatalysis field, but operate
Step is complicated, and reaction time is longer, and technical difficulty is big.Chinese invention issued patents the 201610163670.4th discloses one
Kind different-shape self assembly Cu2The preparation of S nano material is first reacted 2 ~ 6 hours under nitrogen protection, then forged under an inert gas
Burning obtains different-shape self assembly Cu2S nano material, 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.
Summary of the invention
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 material
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 scheme adopted by the invention is that: a kind of Cu of vanadium modification2S self-supporting electrode
The synthetic method of material, comprising the following steps:
(1) foam copper is successively immersed in acetone, hydrochloric acid and water and ethyl alcohol and is cleaned by ultrasonic, is then dried in vacuo, salt
Acid concentration is 1 ~ 5 mol/L；
(2) 12 hydration sodium vanadates are selected and thioacetamide is raw material, weigh certain mass, control vanadium source is rubbed with sulphur source
You than be 1:(1 ~ 10), be dissolved in suitable solvent so that vanadium source concentration be 10 ~ 40 mM, stir 3 ~ 20 min, obtain
Suspension A；
(3) the suspension A being stirred is poured into the water heating kettle of 50 mL polytetrafluoroethyllining linings, step (1) is pre-processed
Foam copper be put into polytetrafluoroethyllining lining after sealing, be subsequently placed in homogeneous reaction instrument and react；
(4) after reaction, reaction kettle being cooled down at room temperature, product deionized water and ethyl alcohol alternately rinse for several times,
Vacuum drying obtains the Cu of vanadium modification2S self-supporting electrode material.
Ultrasonic cleaning described in step (1) is 5 ~ 15 min.
Vacuum drying described in step (1) is 5 ~ 15 h of vacuum drying at 20 ~ 40 DEG C.
Solvent described in step (2) is one or more of deionized water, dehydrated alcohol, methanol, ethylene glycol.
Solvent thermal reaction temperature described in step (3) is 70 ~ 200 DEG C, and the reaction time is 1 ~ 30 h.
Vacuum drying described in step (4) is 3 ~ 15 h of vacuum drying at 20 ~ 40 DEG C.
Compared with prior art, the present invention can obtain following the utility model has the advantages that
(1) this method directly synthesizes final product using a step solvent thermal reaction, has low synthesis temperature, operation
Simple 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 big
Large-scale production.
(2) Cu of the vanadium modification of this method preparation2S self-supporting electrode material, pattern is uniform, 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.
Detailed description of the invention
Fig. 1 is the Cu of vanadium modification prepared by the embodiment of the present invention 32X-ray diffraction (XRD) figure of S self-supporting electrode material
Spectrum；
Fig. 2 is the Cu of vanadium modification prepared by the embodiment of the present invention 32The scanning electron microscope (SEM) of S self-supporting electrode material is shone
Piece；
Fig. 3 is the Cu of vanadium modification prepared by the embodiment of the present invention 32The linear sweep voltammetry (LSV) of S self-supporting electrode material
Performance test figure.
Specific embodiment
With reference to the accompanying drawing and specific embodiment the invention will be described in further detail, but the present invention is not limited to
Following embodiment.
Embodiment 1:
(1) foam copper of (2 × 5) cm is immersed in the hydrochloric acid for being cleaned by ultrasonic 5 min in acetone, being immersed in 1 mol/L again
In carry out ultrasonic cleaning 5 min, finally respectively with ethyl alcohol replace with deionized water rinse 3 times, 5 h are dried in vacuo at 20 DEG C
After the foam copper that obtains that treated；
(2) 12 hydration sodium vanadates are chosen and thioacetamide is raw material, taking 12 hydration sodium vanadates is 0.2mmol, control
The molar ratio of vanadium source processed and sulphur source is 1:1, while being added in 20 ml dehydrated alcohols, and 3 min of magnetic agitation is obtained at room temperature
Suspension A；
(3) suspension A and step (1) the pretreated foam copper being stirred is put into 50 mL polytetrafluoroethyllining linings
Middle sealing 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 reacting and terminating, cool down, product deionized water and ethyl alcohol alternately rinse 3 times, then vacuum at 20 DEG C
Dry 5 h obtain a kind of Cu of vanadium modification2S self-supporting electrode material.
Embodiment 2:
(1) foam copper of (2 × 5) cm is immersed in the hydrochloric acid for being cleaned by ultrasonic 5 min in acetone, being immersed in 2 mol/L again
In carry out ultrasonic cleaning 5 min, finally respectively with ethyl alcohol replace with deionized water rinse 3 times, 10 h are dried in vacuo at 20 DEG C
After the foam copper that obtains that treated；
(2) 12 hydration sodium vanadates are chosen and thioacetamide is raw material, taking 12 hydration sodium vanadates is 0.4mmol, control
The molar ratio of vanadium source processed and sulphur source is 1:1, while being added in the mixed liquor of 25 ml dehydrated alcohols and water, at room temperature magnetic force
It stirs 5 min and obtains suspension A；
(3) suspension A and step (1) the pretreated foam copper being stirred is put into 50 mL polytetrafluoroethyllining linings
Middle sealing 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 reacting and terminating, cool down, product deionized water and ethyl alcohol alternately rinse 3 times, then vacuum at 20 DEG C
Dry 10 h obtain the Cu of vanadium modification2S self-supporting electrode material.
Embodiment 3:
(1) foam copper of (2 × 5) cm is immersed in and is cleaned by ultrasonic 5 min in acetone, is immersed in the hydrochloric acid of 3mol/L again
10 min of ultrasonic cleaning are carried out, finally replace flushing 3 times with deionized water with ethyl alcohol respectively, after 5 h are dried in vacuo at 30 DEG C
The foam copper that obtains that treated；
(2) 12 hydration sodium vanadates are chosen and thioacetamide is raw material, taking 12 hydration sodium vanadates is 0.8 mmol, control
The molar ratio of vanadium source processed and sulphur source is 1:2, while being added in 30 ml methanol, and 10 min of magnetic agitation is hanged at room temperature
Turbid A；
(3) suspension A and step (1) the pretreated foam copper being stirred is put into 50 mL polytetrafluoroethyllining linings
Middle sealing 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 reacting and terminating, cool down, product deionized water and ethyl alcohol alternately rinse 3 times, then vacuum at 30 DEG C
Dry 5 h obtain the Cu of vanadium modification2S self-supporting electrode material.
The Cu of vanadium modification manufactured in the present embodiment2S self-supporting electrode material, 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 vanadium and are present in material in the form adulterated.
It can be seen that the sample is in spherical distribution from the SEM figure of Fig. 2, pattern is uniform.
It is 10 mA/cm that the sample be can be seen that from the linear sweep voltammetry figure of Fig. 3 in current density2When, it has
280 mV low overpotential, 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) foam copper of (2 × 5) cm is immersed in the hydrochloric acid for being cleaned by ultrasonic 5 min in acetone, being immersed in 3 mol/L again
In carry out ultrasonic cleaning 13 min, finally respectively with ethyl alcohol replace with deionized water rinse 3 times, be dried in vacuo 10 at 30 DEG C
The foam copper that obtains that treated after h；
(2) 12 hydration sodium vanadates are chosen and thioacetamide is raw material, taking 12 hydration sodium vanadates is 1.2 mmol, control
The molar ratio of vanadium source processed and sulphur source is 1:6, while being added in 30 ml dehydrated alcohols, and 15 min of magnetic agitation is obtained at room temperature
To suspension A；
(3) suspension A and step (1) the pretreated foam copper being stirred is put into 50 mL polytetrafluoroethyllining linings
Middle sealing 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 reacting and terminating, cool down, product deionized water and ethyl alcohol alternately rinse 3 times, then vacuum at 30 DEG C
Dry 10 h obtain the Cu of vanadium modification2S self-supporting electrode material.
Embodiment 5:
(1) foam copper of (2 × 5) cm is immersed in the hydrochloric acid for being cleaned by ultrasonic 5 min in acetone, being immersed in 5 mol/L again
In carry out ultrasonic cleaning 15 min, finally respectively with ethyl alcohol replace with deionized water rinse 3 times, be dried in vacuo 15 at 40 DEG C
The foam copper that obtains that treated after h；
(2) 12 hydration sodium vanadates are chosen and thioacetamide is raw material, taking 12 hydration sodium vanadates is 0.5 mmol, control
The molar ratio of vanadium source processed and sulphur source is 1:10, while being added in 40 ml ethylene glycol, and 20 min of magnetic agitation is obtained at room temperature
Suspension A；
(3) suspension A and step (1) the pretreated foam copper being stirred is put into 50 mL polytetrafluoroethyllining linings
Middle sealing 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 reacting and terminating, cool down, product deionized water and ethyl alcohol alternately rinse 3 times, then vacuum at 40 DEG C
Dry 15 h obtain the Cu of vanadium modification2S self-supporting electrode material.
Claims (7)
1. a kind of Cu of vanadium modification2The synthetic method of S self-supporting electrode material, which comprises the following steps:
Clean foam copper immerses to vanadium source concentration be 10 ~ 40 mM, vanadium source and sulphur source molar ratio are 1:(1 ~ 10) suspension
In, it carries out solvent thermal reaction and obtains the Cu of vanadium modification sufficiently after reaction2S self-supporting electrode material；The vanadium source is 12 water
Close sodium vanadate；The sulphur source is thioacetamide；Solvent is one of deionized water, dehydrated alcohol, methanol, ethylene glycol or more
Kind；Solvent thermal reaction temperature is 70 ~ 200 DEG C, and the reaction time is 1-30 h.
2. a kind of Cu of vanadium modification according to claim 12The synthetic method of S self-supporting electrode material, which is characterized in that
Foam copper is pre-processed, foam copper is successively immersed in acetone, hydrochloric acid and water and ethyl alcohol and is cleaned by ultrasonic, it is dry, it obtains clean
Net foam copper.
3. a kind of Cu of vanadium modification according to claim 12The synthetic method of S self-supporting electrode material, which is characterized in that
After reaction, it is down to room temperature to reaction system, wash products are dry, obtain the Cu of clean vanadium modification2S self-supporting electrode
Material.
4. the Cu of described in any item a kind of vanadium modifications according to claim 1 ~ 32The synthetic method of S self-supporting electrode material, it is special
Sign is that specific steps include:
1) foam copper is successively immersed 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) 12 hydration sodium vanadates are selected and thioacetamide is raw material, weigh certain mass, control vanadium source and sulphur source molar ratio
For 1:(1 ~ 10), be dissolved in suitable solvent so that vanadium source concentration be 10 ~ 40 mM, 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 the pretreated foam of step 1)
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 material.
5. a kind of Cu of vanadium modification according to claim 42The synthetic method of S self-supporting electrode material, which is characterized in that
Ultrasonic cleaning described in step 1) is 5 ~ 15 min.
6. a kind of Cu of vanadium modification according to claim 42The synthetic method of S self-supporting electrode material, which is characterized in that
Vacuum drying described in step 1) is 5 ~ 15 h of vacuum drying at 20 ~ 40 DEG C；Vacuum drying described in step 4) is 20 ~ 40 DEG C
3 ~ 15 h of lower vacuum drying.
7. the Cu for the vanadium modification that any one of claim 1 ~ 6 obtains2S self-supporting electrode material.
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| 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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| CN105024071B (en) * | 2015-06-24 | 2018-03-02 | 三峡大学 | A kind of Cu2S/Cu lithium ion battery negative materials and preparation method |
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