CN108325539A - A kind of Ni of the rodlike vanadium modification for being self-assembled into flower ball-shaped3S2The synthetic method of elctro-catalyst - Google Patents
A kind of Ni of the rodlike vanadium modification for being self-assembled into flower ball-shaped3S2The synthetic method of elctro-catalyst Download PDFInfo
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- CN108325539A CN108325539A CN201810212194.XA CN201810212194A CN108325539A CN 108325539 A CN108325539 A CN 108325539A CN 201810212194 A CN201810212194 A CN 201810212194A CN 108325539 A CN108325539 A CN 108325539A
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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
- B01J27/043—Sulfides with iron group metals or platinum group metals
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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
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- 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 invention discloses a kind of Ni of the rodlike vanadium modification for being self-assembled into flower ball-shaped3S2The synthetic method of elctro-catalyst, includes the following steps：It is 1 that clean nickel foam, which is immersed a concentration of 5 ~ 30 mM in vanadium source, vanadium source and sulphur source molar ratio,:（0.5~12）Suspension in, carry out microwave solvent thermal response, fully reaction after, obtain it is rodlike be self-assembled into flower ball-shaped vanadium modification Ni3S2Electrocatalyst materials.This method is easy to operate, and reaction condition is mild, time-consuming short, and the Ni for the rodlike vanadium modification for being self-assembled into flower ball-shaped prepared3S2Product purity is high, and morphology and size is uniform.To achieve the goals above, the present invention uses following technical scheme.
Description
Technical field
The invention belongs to new energy materials preparation fields, and in particular to it is a kind of it is rodlike be self-assembled into flower ball-shaped vanadium modification
Ni3S2The synthetic method of elctro-catalyst.
Background technology
Electro-catalysis water-splitting technology is the emerging technology of a field of energy environment, such as carbide, phosphide, sulfide
Substance has excellent electrocatalysis characteristic, the extensive concern of people is received, wherein with WS2、MoS2For representative species, have excellent
Hydrogen activity is produced in different electro-catalysis.But currently, water oxygen is turned to the ratedeterming step in water splitting processes, still restrict the whole of water-splitting
A process.Currently, most production oxygen elctro-catalysts still have high overpotential, and cost is higher, limits large-scale use.
Ni3S2Material is since continuous Ni-Ni keys network is through total, so it has intrinsic metallic character.Conductance
Rate height, cheap Ni3S2It is widely used in many fields.The Ni prepared reported at present3S2Material morphology
Including sheet, flower pattern, rodlike etc..
Chinese invention issued patents the 201610552386.6th disclose a kind of negative electrode of lithium ion battery GO-PANT-
Ni3S2The preparation method of composite material, but operating procedure is complicated, and reaction time is longer, technical difficulty is big.Chinese invention is public
It accuses patent the 201610252105.5th and discloses a kind of three nickel of array type curing-carbon nano-tube combination electrode and its preparation side
Method and application, are first reacted with hydro-thermal method, then to obtain a kind of three nickel of array type curing-carbon nanotube multiple for heat-treating methods
Composite electrode material, reaction time is long, severe reaction conditions, and cost is big.Chinese invention issued patents the 201310320738.1st
A kind of electrolysis aquatic products oxygen composite catalyzing electrode and preparation method thereof number is disclosed, has been prepared with rodlike using the method for hydro-thermal
Ni (OH)2/ Ni3S2Combination electrode, but material overpotential is larger, can not use under conditions of high current, catalytic activity is poor.
This patent is by vanadium-based materials and Ni3S2Material is combined, with special appearance, efficient, cheap for producing
And preparation process simply analyses oxygen elctro-catalyst and has great importance.
Invention content
This patent is directed to the deficiency of above-mentioned material, proposes a kind of Ni of the rodlike vanadium modification for being self-assembled into flower ball-shaped3S2Electricity is urged
The synthetic method of agent, this method is easy to operate, and reaction condition is mild, takes short, and for preparing rodlike is self-assembled into bouquet
The Ni of the vanadium modification of shape3S2Product purity is high, and morphology and size is uniform.To achieve the goals above, the present invention uses following technology
Scheme.
To achieve the goals above, the technical solution adopted in the present invention is：A kind of rodlike vanadium for being self-assembled into flower ball-shaped
The Ni of modification3S2The method of elctro-catalyst, includes the following steps：
（1）Pending nickel foam is soaked into acetone and is cleaned by ultrasonic, then nickel foam is immersed in the hydrochloric acid of 0.5 ~ 4 mol/L
In be cleaned by ultrasonic, finally replace flushing with deionized water with ethyl alcohol respectively, pretreated nickel foam obtained after vacuum drying；
（2）Vanadium source and the sulphur source of certain mass are weighed, control vanadium source is 1 with sulphur source molar ratio:（0.5~12）, it is dissolved in suitable
In solvent so that a concentration of 5 ~ 30 mM in vanadium source, stir 3 ~ 20 min, obtain suspension A；
（3）The suspension A and step that will be stirred（1）In pretreated nickel foam be placed in microwave hydrothermal instrument and react；
（4）After reaction, product deionized water and ethyl alcohol are alternately rinsed for several times, it is rodlike certainly to obtain one kind for vacuum drying
It is assembled into the Ni of the vanadium modification of flower ball-shaped3S2Electrocatalyst materials.
Step（1）The ultrasonic cleaning is 5 ~ 15 min.
Step（1）The vacuum drying is 3 ~ 15 h of vacuum drying at 10 ~ 60 DEG C.
Step（2）The vanadium source is vanadic anhydride, sodium metavanadate, sodium vanadate, 12 hydration sodium vanadates, ammonium metavanadate
And one or more of vanadyl acetylacetonate.
Step（2）The sulphur source is thiocarbamide, thioacetamide, vulcanized sodium, sodium oiethyl dithiocarbamate and sulphur
One or more of simple substance.
Step（2）The solvent is one or more of deionized water, absolute ethyl alcohol, methanol, ethylene glycol.
Step（3）The reaction temperature is 60 ~ 120 DEG C, and power is 200 ~ 400 W, and the reaction time is 0.5 ~ 2 h.
Step（4）The vacuum drying is 3 ~ 15 h of vacuum drying at 10 ~ 60 DEG C.
The present invention also provides the Ni of the uniform vanadium modification of pattern made from the above method3S2Electrocatalyst materials.
Compared with prior art, the present invention can obtain following advantageous effect：
（1）The present invention directly synthesizes the Ni of the uniform vanadium modification of pattern using microwave solvothermal method3S2Electrocatalyst materials close
It is low at temperature, generated time is short, raw material sources are wide, at low cost, environmentally friendly, be suitble to large-scale production.
（2）The Ni of vanadium modification prepared by the present invention3S2Electrocatalyst materials obtain the rodlike of special construction and are self-assembled into flower
The Ni of spherical vanadium modification3S2Electrocatalyst materials increase the specific surface area of material so that the active site of material increases
It is more, and the unique three-dimensional porous structure of foam nickel base, the contact resistance of material is reduced, the transmittability of charge is improved,
The chemical property of material is set to enhance.
（3）The present invention greatly improves the catalysis of catalyst by introducing suitable vanadium source, the synergistic effect that the two generates
Activity can be used as a kind of excellent electro-catalysis production oxygen elctro-catalyst, in 10 mA/cm2Current density under, overpotential can be low
To 180 mV, in 100 mA/cm2Current density under, overpotential can be down to 440 mV.
Description of the drawings
Fig. 1 is the Ni of the vanadium modification being grown in nickel foam prepared by the embodiment of the present invention 23S2The X- of electrocatalyst materials
X ray diffraction（XRD）Collection of illustrative plates；
Fig. 2 is the Ni of the vanadium modification being grown in nickel foam prepared by the embodiment of the present invention 23S2The amplification of electrocatalyst materials
700 times of scanning electron microscope（SEM）Photo；
Fig. 3 is the Ni of the vanadium modification being grown in nickel foam prepared by the embodiment of the present invention 23S2The amplification of electrocatalyst materials
4000 times of scanning electron microscope（SEM）Photo；
Fig. 4 is the Ni of the vanadium modification being grown in nickel foam prepared by the embodiment of the present invention 23S2The amplification of electrocatalyst materials
20000 times of scanning electron microscope（SEM）Photo；
Fig. 5 is the Ni of the vanadium modification being grown in nickel foam prepared by the embodiment of the present invention 23S2The linear of electrocatalyst materials is swept
Retouch volt-ampere（LSV）Performance test figure.
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 nickel foam of cm, which is immersed in successively in acetone, hydrochloric acid, is cleaned by ultrasonic 5 min, then respectively use ethyl alcohol with
Deionized water is alternately rinsed 3 times, and concentration of hydrochloric acid is 0.5 mol/L, is then dried in vacuo at 10 DEG C after 3 h after obtaining processing
Nickel foam；
（2）It is raw material to choose vanadic anhydride and thiocarbamide, and it is 0.075 mmol to take vanadyl acetylacetonate, controls vanadium source and sulphur source
Molar ratio is 1：0.5, while being added in 15 ml absolute ethyl alcohols, 3 min of magnetic agitation obtains suspension A at room temperature；
（3）The suspension A and step that will be stirred（1）In the metallic nickel handled well be positioned in microwave reaction instrument, in temperature
It is 60 DEG C, power is 30 min of solvent thermal reaction under 200 W,
（4）After reaction terminates, cools down, product deionized water and ethyl alcohol alternately rinse 3 times, are then dried in vacuo 3 at 10 DEG C
H obtains a kind of Ni of the rodlike vanadium modification for being self-assembled into flower ball-shaped3S2Electrocatalyst materials.
Embodiment 2：
（1）It will（2×5）The nickel foam of cm, which is immersed in successively in acetone, hydrochloric acid, is cleaned by ultrasonic 5 min, then respectively use ethyl alcohol with
Deionized water is alternately rinsed 3 times, and concentration of hydrochloric acid is 1 mol/L, is then dried in vacuo at 10 DEG C after 5 h and is obtained that treated
Nickel foam；
（2）It is raw material to choose vanadic anhydride and thioacetamide, and it is 0.15 mmol to take vanadyl acetylacetonate, control vanadium source with
The molar ratio of sulphur source is 1：1, while being added in 15 ml absolute ethyl alcohols, 5 min of magnetic agitation obtains suspension A at room temperature；
（3）The suspension A and step that will be stirred（1）In the metallic nickel handled well be positioned in microwave reaction instrument, in temperature
It is 80 DEG C, power is 60 min of solvent thermal reaction under 200 W,
（4）After reaction terminates, cools down, product deionized water and ethyl alcohol alternately rinse 3 times, are then dried in vacuo 3 at 20 DEG C
H obtains a kind of Ni of the rodlike vanadium modification for being self-assembled into flower ball-shaped3S2Electrocatalyst materials.
The Ni of vanadium modification manufactured in the present embodiment3S2Electrocatalyst materials, as can be seen from Figure 1 X-ray powder diffraction peak
The position of appearance is expressed as Ni3S2, occur almost without other peaks, show that V is present in doped forms in material.
The Ni modified from 700 times of SEM it can be seen from the figure that vanadium of amplification of Fig. 23S2Electrocatalyst materials homoepitaxial is in foam
Nickel surface can be seen that the Ni that vanadium is modified from Fig. 3 and Fig. 4 SEM photographs3S2Electrocatalyst materials, which are bar-like, is self-assembled into flower ball-shaped
Array, from the linear sweep voltammetry it can be seen from the figure that of Fig. 5, which is 10 mA/cm in current density2When, it has
Overpotential low 180 mV, in 100 mA/cm2Current density under, with the low overpotential of 440 mV, it is good to show that material has
Good electro-catalysis oxygen evolution activity.
Embodiment 3：
（1）It will（2×5）The nickel foam of cm, which is immersed in successively in acetone, hydrochloric acid, is cleaned by ultrasonic 10 min, then respectively use ethyl alcohol with
Deionized water is alternately rinsed 3 times, and concentration of hydrochloric acid is 2 mol/L, is then dried in vacuo at 20 DEG C after 10 h and is obtained that treated
Nickel foam；
（2）It is raw material to choose sodium metavanadate and sulphur simple substance, and it is 0.3 mmol to take vanadyl acetylacetonate, controls rubbing for vanadium source and sulphur source
You are than being 1：4, while being added in 15 ml absolute ethyl alcohols, 10 min of magnetic agitation obtains suspension A at room temperature；
（3）The suspension A and step that will be stirred（1）In the metallic nickel handled well be positioned in microwave reaction instrument, in temperature
It is 100 DEG C, power is 90 min of solvent thermal reaction under 300 W,
（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 a kind of Ni of the rodlike vanadium modification for being self-assembled into flower ball-shaped3S2Electrocatalyst materials.
Embodiment 4：
（1）It will（2×5）The nickel foam of cm, which is immersed in successively in acetone, hydrochloric acid, is cleaned by ultrasonic 10 min, then respectively use ethyl alcohol with
Deionized water is alternately rinsed 3 times, and concentration of hydrochloric acid is 2.5 mol/L, is then dried in vacuo at 40 DEG C after 10 h after obtaining processing
Nickel foam；
（2）It is raw material to choose sodium vanadate and diethyl thiocarbamic acid, and it is 0.4 mmol, control vanadium source to take vanadyl acetylacetonate
Molar ratio with sulphur source is 1：5, while being added in the mixture of 20 ml absolute ethyl alcohols and water, magnetic agitation 15 at room temperature
Min obtains suspension A；
（3）The suspension A and step that will be stirred（1）In the metallic nickel handled well be positioned in microwave reaction instrument, in temperature
It is 100 DEG C, power is that microwave hydrothermal reacts 90 min under 300 W,
（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
10 h obtain a kind of Ni of the rodlike vanadium modification for being self-assembled into flower ball-shaped3S2Electrocatalyst materials.
Embodiment 5：
（1）It will（2×5）The nickel foam of cm, which is immersed in successively in acetone, hydrochloric acid, is cleaned by ultrasonic 15 min, then respectively use ethyl alcohol with
Deionized water is alternately rinsed 3 times, and concentration of hydrochloric acid is 3 mol/L, is then dried in vacuo at 40 DEG C after 15 h and is obtained that treated
Nickel foam；
（2）It is raw material to choose 12 hydration sodium vanadates and vulcanized sodium, and it is 0.4 mmol to take vanadyl acetylacetonate, controls vanadium source and sulphur
The molar ratio in source is 1：10, while being added in 20 ml ethylene glycol, 15 min of magnetic agitation obtains suspension A at room temperature；
（3）The suspension A and step that will be stirred（1）In the metallic nickel handled well be positioned in microwave reaction instrument, in temperature
It is 120 DEG C, power is 120 min of solvent thermal reaction under 400 W,
（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 a kind of Ni of the rodlike vanadium modification for being self-assembled into flower ball-shaped3S2Electrocatalyst materials.
Embodiment 6：
（1）It will（2×5）The nickel foam of cm, which is immersed in successively in acetone, hydrochloric acid, is cleaned by ultrasonic 15 min, then respectively use ethyl alcohol with
Deionized water is alternately rinsed 3 times, and concentration of hydrochloric acid is 4 mol/L, is then dried in vacuo at 60 DEG C after 15 h and is obtained that treated
Nickel foam；
（2）It is raw material to choose vanadyl acetylacetonate and thioacetamide, and it is 0.9 mmol to take vanadyl acetylacetonate, control vanadium source with
The molar ratio of sulphur source is 1：12, while being added in the mixed solution of 30 ml ethylene glycol and water, magnetic agitation 20 at room temperature
Min obtains suspension A；
（3）The suspension A and step that will be stirred（1）In the metallic nickel handled well be positioned in microwave reaction instrument, in temperature
It is 120 DEG C, power is 120 min of solvent thermal reaction under 400 W,
（4）After reaction terminates, cools down, product deionized water and ethyl alcohol alternately rinse 3 times, are then dried in vacuo at 60 DEG C
15 h obtain a kind of Ni of the rodlike vanadium modification for being self-assembled into flower ball-shaped3S2Electrocatalyst materials.
Claims (10)
1. a kind of Ni of the rodlike vanadium modification for being self-assembled into flower ball-shaped3S2, which is characterized in that the flower ball-shaped with micron order size
Structure, the flower ball-shaped structure are the Ni modified by acicular vanadium3S2The flower ball-shaped structure clustered round.
2. a kind of Ni of the rodlike vanadium modification for being self-assembled into flower ball-shaped3S2The method of elctro-catalyst, which is characterized in that including following
Step：
It is 1 that clean nickel foam, which is immersed a concentration of 5 ~ 30 mM in vanadium source, vanadium source and sulphur source molar ratio,:（0.5~12）Suspension
In, microwave solvent thermal response is carried out, fully after reaction, obtains the Ni of the rodlike vanadium modification for being self-assembled into flower ball-shaped3S2Elctro-catalyst
Material.
3. a kind of Ni of rodlike vanadium modification for being self-assembled into flower ball-shaped according to claim 23S2The method of elctro-catalyst,
It is characterized in that, the vanadium source is vanadic anhydride, sodium metavanadate, sodium vanadate, 12 hydration sodium vanadates, ammonium metavanadate, acetyl
It is one or more in acetone vanadyl.
4. a kind of Ni of rodlike vanadium modification for being self-assembled into flower ball-shaped according to claim 23S2The method of elctro-catalyst,
It is characterized in that, the sulphur source is one in thiocarbamide, thioacetamide, vulcanized sodium, sodium oiethyl dithiocarbamate, sulphur simple substance
Kind is a variety of.
5. a kind of Ni of rodlike vanadium modification for being self-assembled into flower ball-shaped according to claim 23S2The method of elctro-catalyst,
It is characterized in that, the solvent of the suspension is one or more in deionized water, absolute ethyl alcohol, methanol, ethylene glycol.
6. a kind of Ni of rodlike vanadium modification for being self-assembled into flower ball-shaped according to claim 23S2The method of elctro-catalyst,
It is characterized in that, step 3）The reaction temperature of the microwave solvent thermal response is 60 ~ 120 DEG C, and power is 200 ~ 400 W, reaction
Time is 0.5 ~ 2 h.
7. a kind of Ni of rodlike vanadium modification for being self-assembled into flower ball-shaped according to claim 23S2The method of elctro-catalyst,
It is characterized in that, being pre-processed to nickel foam, nickel foam is immersed in successively in acetone, hydrochloric acid and is cleaned by ultrasonic, then with ethyl alcohol,
Deionized water is alternately rinsed, and clean nickel foam is obtained after dry.
8. a kind of Ni of rodlike vanadium modification for being self-assembled into flower ball-shaped according to claim 23S2The method of elctro-catalyst,
It is characterized in that, after reaction, product is rinsed, and it is dry, obtain the Ni of the rodlike vanadium modification for being self-assembled into flower ball-shaped3S2Electricity is urged
Agent material.
9. according to a kind of Ni of the rodlike vanadium modification for being self-assembled into flower ball-shaped of claim 2 ~ 8 any one of them3S2Elctro-catalyst
Method, which is characterized in that specific steps include：
1）Pending nickel foam is soaked into acetone and is cleaned by ultrasonic, then nickel foam is immersed in the hydrochloric acid of 0.5 ~ 4 mol/L
In be cleaned by ultrasonic, finally replace flushing with deionized water with ethyl alcohol respectively, pretreated nickel foam obtained after vacuum drying；
The ultrasonic cleaning is 5 ~ 15 min；
2）Vanadium source and the sulphur source of certain mass are weighed, control vanadium source is 1 with sulphur source molar ratio:（0.5~12）, it is dissolved in suitable
In solvent so that a concentration of 5 ~ 30 mM in vanadium source, stir 3 ~ 20 min, obtain suspension A；
3）The suspension A and step 1 that will be stirred）In pretreated nickel foam be placed in microwave hydrothermal instrument and react；
4）After reaction, product deionized water and ethyl alcohol are alternately rinsed for several times, vacuum drying, is obtained a kind of rodlike from group
Dress up the Ni of the vanadium modification of flower ball-shaped3S2Electrocatalyst materials.
10. a kind of Ni of rodlike vanadium modification for being self-assembled into flower ball-shaped according to claim 93S2The method of elctro-catalyst,
It is characterized in that, step 1）, step 4）The vacuum drying is 3 ~ 15 h of vacuum drying at 10 ~ 60 DEG C.
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