CN105483751A - Efficient Ni-S-Mo hydrogen evolution electrode and preparation method thereof - Google Patents
Efficient Ni-S-Mo hydrogen evolution electrode and preparation method thereof Download PDFInfo
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- CN105483751A CN105483751A CN201510897517.XA CN201510897517A CN105483751A CN 105483751 A CN105483751 A CN 105483751A CN 201510897517 A CN201510897517 A CN 201510897517A CN 105483751 A CN105483751 A CN 105483751A
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- C25—ELECTROLYTIC OR ELECTROPHORETIC PROCESSES; APPARATUS THEREFOR
- C25B—ELECTROLYTIC OR ELECTROPHORETIC PROCESSES FOR THE PRODUCTION OF COMPOUNDS OR NON-METALS; APPARATUS THEREFOR
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- C25B11/073—Electrodes formed of electrocatalysts on a substrate or carrier characterised by the electrocatalyst material
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- 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
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- C25B1/04—Hydrogen or oxygen by electrolysis of water
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- C25D—PROCESSES FOR THE ELECTROLYTIC OR ELECTROPHORETIC PRODUCTION OF COATINGS; ELECTROFORMING; APPARATUS THEREFOR
- C25D15/00—Electrolytic or electrophoretic production of coatings containing embedded materials, e.g. particles, whiskers, wires
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- C25D9/00—Electrolytic coating other than with metals
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Abstract
The invention discloses an efficient Ni-S-Mo hydrogen evolution electrode and a preparation method thereof. The method comprises the steps of removing oxidation layers and grease substances on the surface of a nickel sheet or foamed nickel through mechanical grinding, degreasing of an alkali wash mode or an electrolytic mode and acid pickling; depositing Ni, S and Mo on a pretreated conductive base body in an electro-deposition mode. Nanometer molybdenum particles serving as molybdenum sources are uniformly mixed into a clad layer for forming a clad layer structure with the excellent hydrogen evolution ability, the uniform clad layer and the high hydrogen evolution activity. The method has the advantages that the operation is simple, the production cost is low and the structure of the clad layer is firm. The hydrogen evolution catalytic active electrode prepared through the method can be widely used in the alkaline water electrolysis industry.
Description
Technical field
The present invention relates to hydrogen preparation field, be specifically related to a kind of less energy-consumption Ni-S-Mo hydrogen-precipitating electrode and preparation method thereof.
Background technology
The life of modern humans is inseparable with the energy, and the energy is the foundation of the very fast development of modern economy, is also the grand strategy goods and materials of social development simultaneously.Along with the consumption of conventional fossil fuel and the increase of environmental pollution pressure, we are badly in need of needs and tap a new source of energy.That carries out now carrying out now in the new forms of energy studied studying mainly contains hydroelectric resources, nuclear energy, wind energy, biomass energy, sun power, Hydrogen Energy, shale gas, sea energy etc.In numerous new forms of energy, Hydrogen Energy wherein most has development potentiality.
At present, hydrogen producing technology mainly contains four kinds.Be the non-renewable hydrogen obtained by consuming the fossil energies such as coal, oil, Sweet natural gas, one prepares hydrogen by brine electrolysis, and one is solar hydrogen making, also has a kind of method to be biological hydrogen production.
It is reliable, clean that water electrolysis prepares the method for hydrogen.But water electrolysis hydrogen producing is compared to other preparation methods, need higher energy expenditure.Therefore electricity-eating tiger is called as.So the energy consumption reducing water electrolysis hydrogen producing is the target that insider pursues always.In water electrolysis hydrogen producing technology, alkaline water electrode technology is ripe, simple to operate, is widely used at present.The essence of brine electrolysis is chemical energy by electric energy conversion.It is advance large-scale commercial production to need the difficult problem solved that minimizing energy consumption reduces costs.Energy consumption is relevant with the impedance existed in brine electrolysis process.In electrolytic process, three kinds of main impedances are electronic resistance, electrode reaction resistance and transfer impedance.Wherein main electrode reaction resistance size depends on electrode active surface, and the size of electrode active surface is embodied by the liberation of hydrogen of electrode and overpotential for oxygen evolution.Negative electrode produces hydrogen electrode as alkaline water electrolytic, and height and the power that is mechanical, chemical stability of its overpotential of hydrogen evolution have larger impact to system energy consumption and safe and stable operation.
The factor affecting cathode hydrogen evolution electrode materials electrocatalytic hydrogen evolution activity mainly contains two factors, i.e. capacity factor and geometrical factor, and capacity factor is the bond energy of metal-hydrogen key, and the metal with appropriate absorption hydrogen characteristic is easy to form active higher metal alloy; Geometrical factor is specific surface and the surface tissue form of electrode materials.For many years, for overpotential, the raising electrocatalytic hydrogen evolution reducing electrolysis hydrogen-precipitating electrode is active, reduce energy consumption, many Technological research workers, around capacity factor and geometrical factor, develop many new hydrogen evolution electrode materials.
Summary of the invention
In order to solve problems of the prior art, the invention provides a kind of efficient Ni-S-Mo hydrogen-precipitating electrode and preparation method thereof, overcoming hydrogen-precipitating electrode in prior art, to prepare energy expenditure high, the problem of suitability for industrialized production difficulty.
Technical scheme of the present invention is: a kind of efficient Ni-S-Mo hydrogen-precipitating electrode, described electrode adopts nanometer molybdenum particle to originate as molybdenum element, adopt the mode of composite electrodeposition, nanometer molybdenum uniform particles is doped in Catalytic Layer, thus the efficient Ni-S-Mo hydrogen-precipitating electrode containing nanometer molybdenum particle prepared.Described nanometer molybdenum grain diameter is at 5 ~ 100nm.
A preparation method for efficient Ni-S-Mo hydrogen-precipitating electrode, comprises the following steps:
(1) pre-treatment of conductive substrates;
(2) Ni-S middle layer is prepared in galvanic deposit;
(3) Ni-S-Mo Catalytic Layer is prepared in galvanic deposit, obtains Ni-S/Ni-S-Mo electrode.
Described step (1) conductive substrates is nickel plate or nickel foam.
The pretreatment process of described step (1) substrate is:
When matrix is nickel plate, first grinding process is carried out to it, adopt 20 orders and 60 order sand paper herein, clean with deionized water rinsing after polishing; Then alkali cleaning oil removing is carried out to nickel plate, its step is placed in by alkaline wash after thermostat water bath is warming up to 100 DEG C the nickel foil of mechanical workout to put into wherein, constant temperature process 1h, alkaline wash formula is: the sodium hydroxide of massfraction 10%, the sodium carbonate of massfraction 2%; Clean with deionized water rinsing afterwards; Afterwards nickel foil is carried out cleanup acid treatment: put into acid solution and soak 30min, pickle solution collocation method is concentrated hydrochloric acid and deionized water are mixed according to the volume ratio of 1:2; Afterwards with deionized water rinsing until pH is neutral, stand-by;
When matrix is nickel foam, need to carry out electrolytic degreasing; Nickel foam as negative electrode and anode, is positioned in electrolytic solution by priority, respectively electrolysis 15min, and current density is 40mAcm
-2; Electrolyte component is: sodium hydroxide 40gL
-1, sodium carbonate 25gL
-1, sodium phosphate 25gL
-1; Through the electrode of oil removal treatment, be neutral by deionized water rinsing to pH value repeatedly.
The preparation method in described step (2) Ni-S middle layer is:
Adopt galvanic deposit mode, with the conductive substrates handled well for working electrode, Ni plate is to electrode; The composition of Ni-S plating solution is: thiocarbamide 25gL
-1, single nickel salt 100gL
-1, nickelous chloride 30gL
-1; Bath temperature is 20 ~ 30 DEG C; In electroplating process, current density is 20 ~ 30mAcm
-2, depositing time is 10 ~ 25min; Plating terminates rear deionized water rinsing, to remove residual plating solution, obtains Ni-S middle layer after natural air drying.
The preparation method of described step (3) Ni-S-Mo Catalytic Layer is:
Adopt galvanic deposit mode, with the Ni-S electrode prepared for negative electrode, Ni plate is anode; Ni-S-Mo plating solution consists of: single nickel salt 60 ~ 120gL
-1, thiocarbamide 15 ~ 35gL
-1, anhydrous sodium acetate 5 ~ 25gL
-1, Trisodium Citrate 15 ~ 35gL
-1, ammonium chloride 5 ~ 25gL
-1, boric acid 5 ~ 15gL
-1, nanometer molybdenum particle 5 ~ 25gL
-1; Bath temperature is 20 ~ 30 DEG C; In electroplating process, current density is 30 ~ 100mAcm
-2, depositing time is 10 ~ 50min; In electroplating process, for ensureing that Mo particle is uniformly dispersed in deposit fluid, apply the magnetic agitation of certain rotating speed in the bottom of electrolyzer; Plating terminates rear deionized water rinsing, to remove residual plating solution, obtains Ni-S/Ni-S-Mo electrode after natural air drying.
What described galvanic deposit all adopted is three-electrode system.
The molybdenum element that described step (3) deposits derives from nanometer molybdenum particle, and molybdenum grain diameter is at 5 ~ 100nm.
Beneficial effect of the present invention is: electrode specific surface area prepared by (1) the present invention is large, and catalytic hydrogen evolution activity is high.This method utilizes nanometer molybdenum particle to originate as molybdenum element.Utilize the mode of composite electrodeposition, nanometer molybdenum particle has been clipped in coating.The deposition of nanometer molybdenum particle, increases the ratio specific surface area of electrode, thus provides more reactive behavior site for evolving hydrogen reaction.And the introducing of molybdenum element, d electronics synergistic effect can be there is due to the reason of electrode structure in Ni and Mo.Because in coating, Ni content is very high, in certain limit, Mo element can produce synergic catalytic effect with Ni, and the catalytic hydrogen evolution that improve electrode is active.
(2) electrode stability is better.In the present invention, Ni-S middle layer is introduced.The introducing in middle layer, can make the Ni-S-Mo of double electrodeposition and matrix have stronger bonding force.Enhance the adhesive ability of nanometer Mo particle.Thus prevent the obscission of Catalytic Layer in evolving hydrogen reaction process, improve the stability of electrode.
Accompanying drawing explanation
Fig. 1 is the scanning electron microscopic picture of Ni-S/Ni-S-Mo combined electrode prepared by embodiment 1;
Fig. 2 is the electrode of embodiment 1 preparation and the polarization of electrode curve of industrial pure ni; Testing method is linear sweep voltammetry, test condition: three-electrode system, and prepared electrode is working electrode, Ag/AgCl is reference electrode, and platinized platinum is supporting electrode, and electrolytic solution adopts the KOH solution of mass concentration 30%, scanning speed is 1mVS-1, and sweep limit is-1.0V to-1.6V;
Fig. 3 is the time-measuring electric potential graphic representation of prepared electrode and industrial pure ni electrode in embodiment 1; Test condition: keep 300mAcm-2, the continued electrolysis time is 50h;
Fig. 4 is polarization of electrode curve prepared by electrode prepared by electrode, embodiment 3 prepared by electrode, embodiment 2 and embodiment 4 prepared by industrial pure nickel electrode, embodiment 1; Testing method is linear sweep voltammetry, test condition: three-electrode system, and prepared electrode is working electrode, Ag/AgCl is reference electrode, and platinized platinum is supporting electrode, and electrolytic solution adopts the KOH solution of mass concentration 30%, scanning speed is 1mVS-1, and sweep limit is-1.0V to-1.6V.
Embodiment
Described in detail below in conjunction with the embodiment of accompanying drawing to present method.
Embodiment 1
(1) pre-treatment of conductive substrates
Choose the nickel plate cut out.Adopt 20 orders and 60 order sand paper to polish to nickel foil, clean with deionized water rinsing after polishing.Then nickel foil carries out alkali cleaning oil removing, and alkali cleaning deoiling step is first placed in by alkaline wash after thermostat water bath is warming up to 100 DEG C the nickel foil of mechanical workout to put into wherein, constant temperature process 1h.Clean with deionized water rinsing afterwards.Alkaline wash is filled a prescription: the sodium hydroxide of massfraction 10%, the sodium carbonate of massfraction 2%.The nickel foil that oil removal treatment is crossed will again through cleanup acid treatment.Put into acid solution and soak 30min.Pickle solution collocation method is concentrated hydrochloric acid and deionized water are mixed according to the volume ratio of 1:2.After pickling, use deionized water rinsing nickel foil, until PH is neutral, stand-by.
Ni-S electrode is prepared in (2) galvanic deposit
Adopt three-electrode system, carry out primary depositing.The conductive substrates handled well with step (1) is for working electrode, and Ni plate is to electrode; Consisting of of Ni-S plating solution: thiocarbamide 25gL
-1, single nickel salt 100gL
-1, nickelous chloride 30gL
-1.Bath temperature is 25 DEG C.In electroplating process, current density is 25mAcm
-2, depositing time is 15min.Plating terminates rear deionized water rinsing, to remove residual plating solution, obtains Ni-S electrode after natural air drying.
(3) double electrodeposition prepares Ni-S/Ni-S-Mo electrode
After Ni-S electrode prepared by (2) process that obtains, again carry out secondary deposition process.Continue to adopt three-electrode system, the Ni-S electrode obtained with (2) is negative electrode, and Ni plate is anode; Ni-S-Mo plating solution consists of: single nickel salt 80gL
-1, thiocarbamide 25gL
-1, anhydrous sodium acetate 10gL
-1, Trisodium Citrate 30gL
-1, ammonium chloride 15gL
-1, boric acid 8gL
-1, median size is 30nm nanometer molybdenum particle 8.3gL
-1.Bath temperature is 27 DEG C.In electroplating process, current density is 50mAcm
-2, depositing time is 30min.In electroplating process, for ensureing that Mo particle is uniformly dispersed in deposit fluid, carry out the magnetic agitation of suitable rotating speed in the bottom of electrolyzer.Plating terminates rear deionized water rinsing, to remove residual plating solution, obtains Ni-S/Ni-S-Mo electrode after natural air drying.
(4) apparent form of Ni-S/Ni-S-Mo combined electrode
Utilize the pattern of XL30E type environmental scanning electron microscope to the Ni-S/Ni-S-Mo combined electrode prepared to observe, obtain scanning electron microscope (SEM) photo as Fig. 1.
(5) the Hydrogen Evolution Performance test of Ni-S/Ni-S-Mo combined electrode
The Ni-S/Ni-S-Mo combined electrode of the testing method of linear potential sweep to preparation in industrial pure nickel electrode and step (3) is adopted to carry out performance test.Adopt three-electrode system, prepared electrode is working electrode, and Ag/AgCl is reference electrode, and platinized platinum is supporting electrode, and electrolytic solution adopts the KOH solution of mass concentration 30%, and scanning speed is 1mVS
-1, sweep limit is-1.0V to-1.6V.On electrochemical workstation, (PARSTAT2273, PrincetonAppliedResrarch company of the U.S.) tests its Hydrogen Evolution Performance, test result corresponding diagram 2.
(6) stability test of Ni-S/Ni-S-Mo combined electrode
Adopt three-electrode system, prepared electrode is working electrode, Ag/AgCl is reference electrode, platinized platinum is supporting electrode, electrolytic solution adopts the KOH solution of mass concentration 30%, on electrochemical workstation, (PARSTAT2273, PrincetonAppliedResrarch company of the U.S.) tests it at 300mAcm
-2time-measuring electric potential graphic representation under electric current, thus measure its stability, test result corresponding diagram 3.
Embodiment 2
Step (1) is with step (1) in embodiment 1;
Ni-S electrode is prepared in (2) galvanic deposit
Adopt three-electrode system, carry out primary depositing.The conductive substrates handled well with step (1) is for working electrode, and Ni plate is to electrode; Consisting of of Ni-S plating solution: thiocarbamide 25gL
-1, single nickel salt 100gL
-1, nickelous chloride 30gL
-1.Bath temperature is 30 DEG C.In electroplating process, current density is 20mAcm
-2, depositing time is 25min.Plating terminates rear deionized water rinsing, to remove residual plating solution, obtains Ni-S electrode after natural air drying.
(3) double electrodeposition prepares Ni-S/Ni-S-Mo electrode
After Ni-S electrode prepared by (2) process that obtains, again carry out secondary deposition process.Continue to adopt three-electrode system, the Ni-S electrode obtained with (2) is negative electrode, and Ni plate is anode; Ni-S-Mo plating solution consists of: single nickel salt 60gL
-1, thiocarbamide 35gL
-1, anhydrous sodium acetate 5gL
-1, Trisodium Citrate 25gL
-1, ammonium chloride 25gL
-1, boric acid 10gL
-1, the nanometer molybdenum particle 5gL of median size 100nm
-1.Bath temperature is 30 DEG C.In electroplating process, current density is 100mAcm
-2, depositing time is 10min.In electroplating process, for ensureing that Mo particle is uniformly dispersed in deposit fluid, carry out the magnetic agitation of suitable rotating speed in the bottom of electrolyzer.Plating terminates rear deionized water rinsing, to remove residual plating solution, obtains Ni-S/Ni-S-Mo electrode after natural air drying.
(4) the Hydrogen Evolution Performance test of Ni-S/Ni-S-Mo combined electrode
The Ni-S/Ni-S-Mo combined electrode of the testing method of linear potential sweep to preparation in industrial Ni-S-Mo electrode and step (3) is adopted to carry out performance test.Adopt three-electrode system, prepared electrode is working electrode, and Ag/AgCl is reference electrode, and platinized platinum is supporting electrode, and electrolytic solution adopts the KOH solution of mass concentration 30%, and scanning speed is 1mVS
-1, sweep limit is-1.0V to-1.6V.On electrochemical workstation, (PARSTAT2273, PrincetonAppliedResrarch company of the U.S.) tests its Hydrogen Evolution Performance, test result corresponding diagram 4.
Embodiment 3
Step (1) is with step (1) in embodiment 1;
Ni-S electrode is prepared in (2) galvanic deposit
Adopt three-electrode system, carry out primary depositing.The conductive substrates handled well with step (1) is for working electrode, and Ni plate is to electrode; Consisting of of Ni-S plating solution: thiocarbamide 25gL
-1, single nickel salt 100gL
-1, nickelous chloride 30gL
-1.Bath temperature is 25 DEG C.In electroplating process, current density is 30mAcm
-2, depositing time is 10min.Plating terminates rear deionized water rinsing, to remove residual plating solution, obtains Ni-S electrode after natural air drying.
(3) double electrodeposition prepares Ni-S/Ni-S-Mo electrode
After Ni-S electrode prepared by (2) process that obtains, again carry out secondary deposition process.Continue to adopt three-electrode system, the Ni-S electrode obtained with (2) is negative electrode, and Ni plate is anode; Ni-S-Mo plating solution consists of: single nickel salt 100gL
-1, thiocarbamide 15gL
-1, anhydrous sodium acetate 25gL
-1, Trisodium Citrate 15gL
-1, ammonium chloride 10gL
-1, boric acid 5gL
-1, the nanometer molybdenum particle 25gL of median size 5nm
-1.Bath temperature is 20 DEG C.In electroplating process, current density is 70mAcm
-2, depositing time is 50min.In electroplating process, for ensureing that Mo particle is uniformly dispersed in deposit fluid, carry out the magnetic agitation of suitable rotating speed in the bottom of electrolyzer.Plating terminates rear deionized water rinsing, to remove residual plating solution, obtains Ni-S/Ni-S-Mo electrode after natural air drying.
(4) the Hydrogen Evolution Performance test of Ni-S/Ni-S-Mo combined electrode
The Ni-S/Ni-S-Mo combined electrode of the testing method of linear potential sweep to preparation in industrial Ni-S-Mo electrode and step (3) is adopted to carry out performance test.Adopt three-electrode system, prepared electrode is working electrode, and Ag/AgCl is reference electrode, and platinized platinum is supporting electrode, and electrolytic solution adopts the KOH solution of mass concentration 30%, and scanning speed is 1mVS
-1, sweep limit is-1.0V to-1.6V.On electrochemical workstation, (PARSTAT2273, PrincetonAppliedResrarch company of the U.S.) tests its Hydrogen Evolution Performance, test result corresponding diagram 4.
Embodiment 4
Step (1) is with step (1) in embodiment 1;
Ni-S electrode is prepared in (2) galvanic deposit
Adopt three-electrode system, carry out primary depositing.The conductive substrates handled well with step (1) is for working electrode, and Ni plate is to electrode; Consisting of of Ni-S plating solution: thiocarbamide 25gL
-1, single nickel salt 100gL
-1, nickelous chloride 30gL
-1.Bath temperature is 20 DEG C.In electroplating process, current density is 25mAcm
-2, depositing time is 20min.Plating terminates rear deionized water rinsing, to remove residual plating solution, obtains Ni-S electrode after natural air drying.
(3) double electrodeposition prepares Ni-S/Ni-S-Mo electrode
After Ni-S electrode prepared by (2) process that obtains, again carry out secondary deposition process.Continue to adopt three-electrode system, the Ni-S electrode obtained with (2) is negative electrode, and Ni plate is anode; Ni-S-Mo plating solution consists of: single nickel salt 120gL
-1, thiocarbamide 15gL
-1, anhydrous sodium acetate 25gL
-1, Trisodium Citrate 35gL
-1, ammonium chloride 5gL
-1, boric acid 15gL
-1, the nanometer molybdenum particle 10gL of median size 80nm
-1.Bath temperature is 20 DEG C.In electroplating process, current density is 30mAcm
-2, depositing time is 50min.In electroplating process, for ensureing that Mo particle is uniformly dispersed in deposit fluid, carry out the magnetic agitation of suitable rotating speed in the bottom of electrolyzer.Plating terminates rear deionized water rinsing, to remove residual plating solution, obtains Ni-S/Ni-S-Mo electrode after natural air drying.
(4) the Hydrogen Evolution Performance test of Ni-S/Ni-S-Mo combined electrode
The Ni-S/Ni-S-Mo combined electrode of the testing method of linear potential sweep to preparation in industrial Ni-S-Mo electrode and step (3) is adopted to carry out performance test.Adopt three-electrode system, prepared electrode is working electrode, and Ag/AgCl is reference electrode, and platinized platinum is supporting electrode, and electrolytic solution adopts the KOH solution of mass concentration 30%, and scanning speed is 1mVS
-1, sweep limit is-1.0V to-1.6V.On electrochemical workstation, (PARSTAT2273, PrincetonAppliedResrarch company of the U.S.) tests its Hydrogen Evolution Performance, test result corresponding diagram 4.
Although invention has been described by reference to the accompanying drawings above; but the present invention is not limited to above-mentioned embodiment; above-mentioned embodiment is only schematic; be not restrictive; those of ordinary skill in the art is under enlightenment of the present invention; do not departing under the ambit that present inventive concept and claim protect, can also make a lot of form, these all belong within protection scope of the present invention.
Claims (10)
1. an efficient Ni-S-Mo hydrogen-precipitating electrode, it is characterized in that, described electrode adopts nanometer molybdenum particle to originate as molybdenum element, adopts the mode of composite electrodeposition, nanometer molybdenum uniform particles is doped in Catalytic Layer, thus the efficient Ni-S-Mo hydrogen-precipitating electrode containing nanometer molybdenum particle prepared.
2. efficient Ni-S-Mo hydrogen-precipitating electrode according to claim 1, is characterized in that, described nanometer molybdenum grain diameter is at 5 ~ 100nm.
3. a preparation method for efficient Ni-S-Mo hydrogen-precipitating electrode, is characterized in that, comprise the following steps:
(1) pre-treatment of conductive substrates;
(2) Ni-S middle layer is prepared in galvanic deposit;
(3) Ni-S-Mo Catalytic Layer is prepared in galvanic deposit, obtains Ni-S/Ni-S-Mo electrode.
4. the preparation method of a kind of efficient Ni-S-Mo hydrogen-precipitating electrode according to claim 3, it is characterized in that, described step (1) conductive substrates is nickel plate or nickel foam.
5. the preparation method of a kind of efficient Ni-S-Mo hydrogen-precipitating electrode according to claim 3, it is characterized in that, the pretreatment process of described step (1) substrate is:
When matrix is nickel plate, first grinding process is carried out to it, adopt 20 orders and 60 order sand paper herein, clean with deionized water rinsing after polishing; Then carry out alkali cleaning oil removing to nickel plate, its step is placed in by alkaline wash after thermostat water bath is warming up to 100 DEG C the nickel foil of mechanical workout to put into wherein, and constant temperature process 1h is clean with deionized water rinsing afterwards; Afterwards nickel foil is carried out cleanup acid treatment: put into acid solution and soak 30min, afterwards with deionized water rinsing until pH is neutral, stand-by;
When matrix is nickel foam, need to carry out electrolytic degreasing; Nickel foam as negative electrode and anode, is positioned in electrolytic solution by priority, respectively electrolysis 15min, and current density is 40mAcm
-2; Through the electrode of oil removal treatment, be neutral by deionized water rinsing to pH value repeatedly.
6. the preparation method of a kind of efficient Ni-S-Mo hydrogen-precipitating electrode according to claim 5, it is characterized in that, described alkaline wash formula is: the sodium hydroxide of massfraction 10%, the sodium carbonate of massfraction 2%; Described pickle solution collocation method is concentrated hydrochloric acid and deionized water are mixed according to the volume ratio of 1:2; Described electrolyte component is: sodium hydroxide 40gL
-1, sodium carbonate 25gL
-1, sodium phosphate 25gL
-1.
7. the preparation method of a kind of efficient Ni-S-Mo hydrogen-precipitating electrode according to claim 3, it is characterized in that, the preparation method in described step (2) Ni-S middle layer is:
Adopt galvanic deposit mode, with the conductive substrates handled well for working electrode, Ni plate is to electrode; The composition of Ni-S plating solution is: thiocarbamide 25gL
-1, single nickel salt 100gL
-1, nickelous chloride 30gL
-1; Bath temperature is 20 ~ 30 DEG C; In electroplating process, current density is 20 ~ 30mAcm
-2, depositing time is 10 ~ 25min; Plating terminates rear deionized water rinsing, to remove residual plating solution, obtains Ni-S middle layer after natural air drying.
8. the preparation method of a kind of efficient Ni-S-Mo hydrogen-precipitating electrode according to claim 3, it is characterized in that, the preparation method of described step (3) Ni-S-Mo Catalytic Layer is:
Adopt galvanic deposit mode, with the Ni-S electrode prepared for negative electrode, Ni plate is anode; Ni-S-Mo plating solution consists of: single nickel salt 60 ~ 120gL
-1, thiocarbamide 15 ~ 35gL
-1, anhydrous sodium acetate 5 ~ 25gL
-1, Trisodium Citrate 15 ~ 35gL
-1, ammonium chloride 5 ~ 25gL
-1, boric acid 5 ~ 15gL
-1, nanometer molybdenum particle 5 ~ 25gL
-1; Bath temperature is 20 ~ 30 DEG C; In electroplating process, current density is 30 ~ 100mAcm
-2, depositing time is 10 ~ 50min; In electroplating process, for ensureing that Mo particle is uniformly dispersed in deposit fluid, apply the magnetic agitation of certain rotating speed in the bottom of electrolyzer; Plating terminates rear deionized water rinsing, to remove residual plating solution, obtains Ni-S/Ni-S-Mo electrode after natural air drying.
9. the preparation method of a kind of efficient Ni-S-Mo hydrogen-precipitating electrode according to claim 3, is characterized in that: what described galvanic deposit all adopted is three-electrode system.
10. the preparation method of a kind of efficient Ni-S-Mo hydrogen-precipitating electrode according to claim 3, it is characterized in that, the molybdenum element that described step (3) deposits derives from nanometer molybdenum particle, and molybdenum grain diameter is at 5 ~ 100nm.
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| CN105921156A (en) * | 2016-05-05 | 2016-09-07 | 哈尔滨工业大学 | Preparing method for tungsten-sulfur-based photocatalytic material |
| CN108671943A (en) * | 2018-05-11 | 2018-10-19 | 北京化工大学 | A kind of micron of slot structure accelerates the application of bubble spilling in electrode evolving hydrogen reaction |
| CN108914156A (en) * | 2018-08-30 | 2018-11-30 | 合肥工业大学 | A kind of Fe-Co-Mo-P-C system amorphous alloy elctro-catalyst and its preparation method and application |
| CN109110735A (en) * | 2018-10-30 | 2019-01-01 | 长安大学 | A kind of Ni3Se2/MoS2Nuclear shell structure nano liberation of hydrogen material and preparation method thereof |
| CN109537006A (en) * | 2018-11-09 | 2019-03-29 | 厦门理工学院 | A kind of efficient Ni-S-B hydrogen-precipitating electrode and its preparation method and application |
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| CN111286750A (en) * | 2018-12-07 | 2020-06-16 | 湖南工业大学 | Nano hierarchical pore Ti-SiO2Preparation method of/Ni-Mo composite hydrogen evolution electrode |
| CN112626552A (en) * | 2021-01-07 | 2021-04-09 | 兰州大学 | Method for electrodepositing Ni-Fe-Sn-P alloy on surface of foamed nickel |
| CN112680744A (en) * | 2021-01-03 | 2021-04-20 | 杜先明 | Porous nickel-based hydrogen evolution electrode composite material |
| CN113529124A (en) * | 2021-06-09 | 2021-10-22 | 武汉纺织大学 | Electrolytic water cathode material, preparation method thereof and application of cathode material in electrocatalytic hydrogenation reduction of dye |
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| CN113529124A (en) * | 2021-06-09 | 2021-10-22 | 武汉纺织大学 | Electrolytic water cathode material, preparation method thereof and application of cathode material in electrocatalytic hydrogenation reduction of dye |
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| CN114672836A (en) * | 2022-05-12 | 2022-06-28 | 江苏科技大学 | Catalyst hydrogen evolution electrode and preparation method thereof |
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| CN116377501A (en) * | 2023-04-10 | 2023-07-04 | 陕西华秦新能源科技有限责任公司 | Electrocatalytic hydrogen evolution material and preparation method and application thereof |
| CN116377501B (en) * | 2023-04-10 | 2024-01-02 | 陕西华秦新能源科技有限责任公司 | Electrocatalytic hydrogen evolution material and preparation method and application thereof |
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