CN102787329A - Preparation method of efficient Ni-Mo-P/Ni hydrogen evolution electrode - Google Patents
Preparation method of efficient Ni-Mo-P/Ni hydrogen evolution electrode Download PDFInfo
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Abstract
The invention provides a preparation method of an efficient Ni-Mo-P/Ni hydrogen evolution electrode, which belongs to the field of electro-catalysis hydrogen evolution. The method comprises steps as follows: removing an oxide layer and oil matters from the surface of a nickel sheet by mechanical polishing and ultrasonic washing; then plating the surface of the pre-processed nickel sheet by pulse electrodeposition, doping P into an Ni-Mo coating to form an Ni-Mo-P nano-crystalline coating with excellent hydrogen evolution performance, wherein the Ni-Mo-P nano-crystalline coating is plated uniformly and is located between a crystalline state structure and an amorphous state structure. The method is simple and feasible, the production cost is low; and the Ni-Mo-P/Ni hydrogen evolution electrode prepared by the method is not only applicable to electro-catalysis hydrogen evolution in chlorine alkali industry, but also is widely applicable to various catalytic hydrogen evolution fields such as solar hydrogen production by water electrolysis, and water electrolysis industry and the like.
Description
Technical field
The invention belongs to the electrocatalytic hydrogen evolution field, particularly a kind of efficient Ni-Mo-P/Ni hydrogen-precipitating electrode preparation method.
Background technology
Hydrogen Energy cleans as a kind of efficient, and the ideal secondhand energy receive the attention of various countries' researcher always.Electrolysis aquatic products hydrogen is one of important method of ripe at present and cheap preparation hydrogen.It mainly is Rany Ni that the brine electrolysis hydrogen-precipitating electrode of utilization is gone up in industry at present, materials such as soft steel, but have that bath voltage is big, overpotential is higher, energy consumption is excessive and inferior position such as perishable, become the important factor of restriction chlorine industry development.Though greater activity has appearred having both at home and abroad, the hydrogen-precipitating electrode that energy consumption is low, it costs an arm and a leg, and production cost is high.Therefore, research and develop the stable hydrogen-precipitating electrode of a kind of efficient cheapness and have very important realistic meaning and practical value.
Discover that reducing overpotential of hydrogen evolution mainly contains two kinds of methods: the one, improve the specific surface area of electrode, promptly increase the porosity or the surfaceness of electrode, to reduce the real current density of electrode in the electrolytic process; The 2nd, improve the electrochemical activity of electrode itself, promptly seek the new evolving hydrogen material of high catalytic activity.Research shows that transition is the overpotential of hydrogen evolution that metal alloy can reduce metallic substance through synergistic effect.Nickelalloy compares with precious metal as the electrolyzed alkaline water cathode material that cost is low, the preparation method has good electrochemical simply, simultaneously and solidity to corrosion and receive extensive concern preferably.The Ni-Mo alloy is proved to be the best binary alloy of liberation of hydrogen performance in the basic soln.Preparation liberation of hydrogen alloy electrode mainly adopts the simple electro-deposition method of preparation process at present; But exist internal stress big; Coating and matrix adhesive force are not good, and long-term electrolysis is prone to come off etc., and may absorb and get into lattice and lose catalytic activity because of forming hydrogenate or hydrogen during the long-term electrolysis of electrode.In addition, electrode may lose catalytic activity because activeconstituents is oxidized under open-circuit condition.
The domestic in recent years high efficiency to electrolyzed alkaline water catalytic hydrogen evolution electrode has been done a large amount of research with stability.1) Chinese invention patent CN 102127775 A disclose " preparation method of nickel-molybdenum-sulfur hydrogen evolution electrode "; Through preparing Ni-Mo and Ni-S electroplating solution respectively; Adopt the nickel plate to do anode then, nickel foam is made cathode material and is carried out Ni-S, Ni-Mo, Ni-S, four plating of Ni-Mo successively.Advantages such as prepared Ni-Mo-S hydrogen-precipitating electrode has active height, energy consumption is low, cheap, energy-saving effect is obvious.But the liberation of hydrogen coating of this method preparation exists the bonding force between coating and the nickel foam substrate poor simultaneously, and the hydrogen that the coating particle is big, electrolysis produces is prone in nickel foam, pile up and problem such as is difficult to separate out.2) Chinese invention patent CN 101665951 A disclose " process of preparing Ni-W-Fe-La nanocrystalline hydrogen evolution electrode material through pulse electrodeposition ", and this invention is added rare earth element ion La in electroplate liquid
3+, adopt the pulse electrodeposition method on soft steel, to prepare the Ni-W-Fe-La nanocrystalline hydrogen evolution electrode material.This method is evenly fine and close through the coating that adds the REE preparation, stable components, and sticking power is better and have electro catalytic activity and a resistance of oxidation preferably.But the electronegativity of REE is higher, is difficult to from the aqueous solution, reduce get in the alloy layer.
Summary of the invention
The objective of the invention is provides a kind of efficient Ni-Mo-P/Ni hydrogen-precipitating electrode preparation method to the requirement of alkaline electrolysis water electrode.The present invention at first removes materials such as surperficial zone of oxidation of nickel sheet and grease through mechanical grinding, ultrasonic cleaning; Execute in the plating of pretreated nickel sheet surface through pulse electrodeposition then, P mixed in the Ni-Mo coating, form have that the liberation of hydrogen ability is good, coating evenly and the Ni-Mo-P nanocrystalline structure coating between crystalline state and amorphous structure.This preparing method's main advantage is to adopt pulse electrodeposition method acquisition specific surface area very big, and the coating that composition is uniform and stable has good liberation of hydrogen performance.
The objective of the invention is to realize like this: a kind of efficient Ni-Mo-P/Ni hydrogen-precipitating electrode preparation method, its concrete grammar step comprises
(1), the pre-treatment of Ni substrate
At first the Ni sheet is carried out the oxide compound that mechanical grinding is removed the surface, clean up with ultrapure water after making its metal luster; Then respectively in alkali lye and absolute ethyl alcohol ultrasonic respectively concussion 20min and 10min carry out electrochemical deoiling, wherein alkali lye is the mixed aqueous solution of 45g/L sodium sulfate, 45g/L yellow soda ash and 45g/L sodium-chlor; Rinse well with deionized water then, immerse in the ethanol solution for use behind the natural air drying;
(2), pulse electrodeposition prepares the Ni-Mo-P/Ni electrode
Adopt two electrode systems, the Ni substrate of handling well with step (1) is a working electrode, and the Ni plate is a counter electrode.Consisting of of Ni-Mo-P plating bath: 20～60 g/L nickel salt aqueous solutions; 10～50 g/L molybdate aqueous solution; 10～60 g/L ortho phosphorous acid sodium water solutions, 20～150 g/L trisodium citrate aqueous solutions, 10～300 g/L sodium chloride aqueous solutions; The pH value of plating bath is 1～10, and bath temperature is 20～60 ℃.Pulse peak current density is 10～30A/dm
2, the pulse ON time is 0.1～10ms, and pulse turn-off time is 0.5～50ms, and electrodeposition time is 5～300s.Electroplate the end back and use deionized water rinsing,, make the Ni-Mo-P electrode behind the natural air drying to remove residual plating bath.
Wherein said nickel salt is one of them of single nickel salt, nickelous nitrate, nickelous chloride; Molybdate is one of them of Sodium orthomolybdate, ammonium molybdate.
After the present invention adopts technique scheme, mainly contain following advantage:
(1), to adopt with the nickel sheet be substrate, good corrosion resistance can strengthen the binding ability of coating and substrate simultaneously, and elements such as employing nickel and molybdenum is cheap, stable performance under the alkaline condition;
(2), adopt pulse electrodeposition, it is even to obtain composition, particle is thinner, consistency of thickness, the coating that internal stress is little;
(3), adopt P is doped to and form the Ni-Mo-P alloy in the Ni-Mo coating, be half noncrystal, active surface area that can be bigger has also increased the stability of electrode simultaneously.
Adopt the Ni-Mo-P coating based on the nickel sheet of the present invention's preparation to have bigger specific surface area and unique amorphous structure, good liberation of hydrogen performance and stable preferably can be extensively as the electrolyzed alkaline water hydrogen evolution electrode material.
Description of drawings
Fig. 1 is the prepared Ni-Mo-P/Ni coating stereoscan photograph of embodiment 1;
Among the figure: Fig. 1 is the stereoscan photograph of the Ni-Mo-P nano particle of embodiment 1 preparation.
Fig. 2 is the prepared Ni-Mo-P coating of embodiment 2 and the X ray diffracting spectrum of pure nickel sheet;
Among the figure: curve 1 is that embodiment 2 prepared Ni-Mo-P/Ni coating are 2 °/min in sweep velocity, and sweep limit is 30 °～80 ° a X ray diffracting spectrum;
Fig. 3 is the linear time base sweep curve of pure nickel sheet among embodiment 3 prepared Ni-Mo-P/Ni coating and the contrast experiment;
Among the figure: curve 1 is to be working electrode with embodiment 3 prepared Ni-Mo-P/Ni coating; SCE is a reference electrode, and platinized platinum is a counter electrode, and the saturated 6 mol sodium hydroxide solutions of nitrogen are electrolytic solution; Temperature is 30 ℃, and sweep velocity is the linear time base sweep curve under 5 millivolts/second;
Fig. 4 is the prepared time-measuring electric potential graphic representation of Ni-Mo-P coating under 250mA of embodiment 4;
Fig. 4 is the time-measuring electric potential curve that embodiment 4 prepared electrodes are tested on CHI660D electrochemical workstation (Shanghai occasion China instrument company).Test condition: three-electrode system, the aqueous sodium hydroxide solution of 6mol/L are electrolyte solution, and embodiment 4 prepared Ni-Mo-P coating are working electrode, and SCE is a reference electrode, and platinized platinum is a supporting electrode, and sustained current density is 250mA/cm
-2, lasting electrolysis time is 10000s.
Embodiment
Below in conjunction with embodiment, further specify the present invention.
Embodiment 1,
(1), the pre-treatment of Ni substrate
At first the Ni sheet is carried out the oxide compound that mechanical grinding is removed the surface, clean up with ultrapure water after making its metal luster; Then respectively in alkali lye and absolute ethyl alcohol ultrasonic respectively concussion 20min and 10min carry out electrochemical deoiling, wherein alkali lye is the mixed aqueous solution of 45g/L sodium sulfate, 45g/L yellow soda ash and 45g/L sodium-chlor; Rinse well with deionized water then, immerse in the ethanol solution for use behind the natural air drying;
(2), pulse electrodeposition prepares the Ni-Mo-P/Ni electrode
Adopt two electrode systems, the Ni substrate of handling well with step (1) is a working electrode, and the Ni plate is a counter electrode.Consisting of of Ni-Mo-P plating bath: the 40g/L nickel sulfate solution, 30 g/L sodium molybdate aqueous solutions, 10 g/L ortho phosphorous acid sodium water solutions, 150 g/L trisodium citrate aqueous solutions, 200 g/L sodium chloride aqueous solutions, the pH value of plating bath is 8, bath temperature is 20 ℃.Pulse peak current density is 30A/dm
2, the pulse ON time is 1ms, and pulse turn-off time is 10ms, and electrodeposition time is 200s.Electroplate the end back and use deionized water rinsing,, make the Ni-Mo-P electrode behind the natural air drying to remove residual plating bath.
Ni-Mo-P/Ni coating electrode for preparing and pure nickel sheet cutting 1cm
2Obtain ESEM (SEM) photo among Fig. 1 with sem test.
Step (1) is with step (1) among the embodiment 1;
(2), pulse electrodeposition prepares the Ni-Mo-P/Ni electrode
Adopt two electrode systems, the Ni substrate of handling well with step (1) is a working electrode, and the Ni plate is a counter electrode.Consisting of of Ni-Mo-P plating bath: the 20g/L nickel nitrate aqueous solution, 50 g/L sodium molybdate aqueous solutions, 60 g/L ortho phosphorous acid sodium water solutions, 150 g/L trisodium citrate aqueous solutions, 10 g/L sodium chloride aqueous solutions, the pH value of plating bath is 10, bath temperature is 60 ℃.Pulse peak current density is 30A/dm
2, the pulse ON time is 0.1ms, and pulse turn-off time is 0.5ms, and electrodeposition time is 5s.Electroplate the end back and use deionized water rinsing,, make the Ni-Mo-P electrode behind the natural air drying to remove residual plating bath.
Ni-Mo-P/Ni coating electrode for preparing and pure nickel sheet cutting 1cm
2Obtain the X ray diffracting spectrum among Fig. 2 with the XRD test.
Embodiment 3,
Step (1) is with step (1) among the embodiment 1;
(2), pulse electrodeposition prepares the Ni-Mo-P/Ni electrode
Adopt two electrode systems, the Ni substrate of handling well with step (1) is a working electrode, and the Ni plate is a counter electrode.Consisting of of Ni-Mo-P plating bath: 60 g/L nickel chloride aqueous solutions, 10 g/L ammonium molybdate aqueous solutions, 30 g/L ortho phosphorous acid sodium water solutions, 20 g/L trisodium citrate aqueous solutions, 300 g/L sodium chloride aqueous solutions, the pH value of plating bath is 1, bath temperature is 40 ℃.Pulse peak current density is 10A/dm
2, the pulse ON time is 10ms, pulse turn-off time is 50ms, electrodeposition time 300s.Electroplate the end back and use deionized water rinsing,, make the Ni-Mo-P electrode behind the natural air drying to remove residual plating bath;
(3), the performance test of Ni-Mo-P/Ni coating liberation of hydrogen,
Adopting three-electrode system, is electrolyte solution with the aqueous sodium hydroxide solution of 6mol/L, and step (2) preparation Ni-Mo-P/Ni coating is working electrode; SCE is a reference electrode, and platinum filament is a supporting electrode, (CHI660B on electrochemical workstation; Shanghai occasion China instrument company) tests its linear time base sweep volt-ampere curve; Probe temperature is 30 ℃, and scanning speed is 5mV/s, and curve 1 in the test result corresponding diagram 3.
Embodiment 4,
Step (1) is with step (1) among the embodiment 1;
(2), pulse electrodeposition prepares the Ni-Mo-P/Ni electrode
Adopt two electrode systems, the Ni substrate of handling well with step (1) is a working electrode, and the Ni plate is a counter electrode.Consisting of of Ni-Mo-P plating bath: 40 g/L nickel sulfate solutions, 30 g/L ammonium molybdate aqueous solutions, 30 g/L ortho phosphorous acid sodium water solutions, 70 g/L trisodium citrate aqueous solutions, 200 g/L sodium chloride aqueous solutions, the pH value of plating bath is 8, bath temperature is 20 ℃.Pulse peak current density is 20A/dm
2, the pulse ON time is 1ms, and pulse turn-off time is 10ms, and electrodeposition time is 200s.Electroplate the end back and use deionized water rinsing,, make the Ni-Mo-P electrode behind the natural air drying to remove residual plating bath;
(3), the stability test of Ni-Mo-P/Ni coating
Adopt three-electrode system; Aqueous sodium hydroxide solution with 6mol/L is an electrolyte solution; The Ni-Mo-P/Ni coating of step (2) preparation is working electrode, and SCE is a reference electrode, and platinized platinum is a supporting electrode; (CHI660B, Shanghai occasion China instrument company) tests it at 250mA/cm on electrochemical workstation
-2Time-measuring electric potential curve under the electric current, test result corresponding diagram 4.
The contrast experiment:
The preprocessing process of Ni sheet is with embodiment 1 step (1)
Adopting three-electrode system, is electrolyte solution with the aqueous sodium hydroxide solution of 6mol/L, and the pretreated pure nickel sheet of step (1) is a working electrode; SCE is a reference electrode, and platinum filament is a supporting electrode, (CHI660B on electrochemical workstation; Shanghai occasion China instrument company) tests its linear time base sweep volt-ampere curve; Probe temperature is 30 ℃, and scanning speed is 5mV/s, and curve 2 in the test result corresponding diagram 3.
Test-results of the present invention:
(1), can find out by stereoscan photograph (Fig. 1); The Ni-Mo-P/Ni coating surface surface irregularity that the present invention is prepared; Uneven Ni-Mo-P alloying pellet is evenly distributed; Than pure nickel sheet smooth planar surface, obviously increase the coating specific surface area, effectively increase the active site of liberation of hydrogen.
(2), can find out that by XRD figure spectrum (Fig. 2) the prepared Ni-Mo-P/Ni coating XRD of the present invention can find in the XRD of Ni-Mo-P, not occur the diffraction peak of independent Mo, explain that Mo is not an exist singly, but and Ni, P exists with the blended form.The adding of P; Make the Ni-Mo alloy layer form non-crystalline state more easily; In the XRD of Ni-Mo-P coating 44 ~ 45 ° of diffraction peaks of locating to occur wideization; But but not successive broadband but isolating spike is considered grain-size (between 1-l00nm) again, so this coating is the nanometer crystal alloy between crystalline state and non-crystalline state.
(3), can find out by linear time base sweep curve (Fig. 3), the prepared liberation of hydrogen coating electrode of the present invention pure nickel electrode of comparing, Ni-Mo-P/Ni has better liberation of hydrogen performance, when
j=100mA.cm
-2The time, the pure nickel hydrogen-evolution overpotential with respect to saturated calomel is-1.654V, and the hydrogen-evolution overpotential of prepared Ni-Mo-P/ Ni is-1.286V (vs SCE), the nearly 370mv that shuffled explains prepared electrode materials liberation of hydrogen superior performance.
(4), can find out that from Fig. 4 curve result adopting the prepared Ni-based Ni-Mo-P coating electrode of the present invention is 250mA/cm in current density
-2Following continuous current continues electrolysis 10000s, and hydrogen-evolution overpotential is initially-1.422V (vs SCE), and becomes behind the EOT-1.406V (vs SCE), tends to be steady afterwards, has improved 17mV.Can see from testing just the hydrogen-evolution overpotential (250mA/cm after the test
-2Go up not down down), supposition is that the stripping of Mo and the oxide compound reduction of Ni all cause avtive spot to increase, when coating reach stablize after hydrogen-evolution overpotential also just reach stable.Proof adopts the prepared Ni-based Ni-Mo-P coating electrode of the present invention to have stability preferably.
Claims (6)
1. efficient Ni-Mo-P/Ni hydrogen-precipitating electrode preparation method, its concrete grammar step comprises
(1), the pre-treatment of Ni substrate
At first the Ni sheet is carried out the oxide compound that mechanical grinding is removed the surface, clean up with ultrapure water after making its metal luster; Then respectively in alkali lye and absolute ethyl alcohol ultrasonic respectively concussion 20min and 10min carry out electrochemical deoiling, wherein alkali lye is the mixed aqueous solution of 45g/L sodium sulfate, 45g/L yellow soda ash and 45g/L sodium-chlor; Rinse well with deionized water then, immerse in the ethanol solution for use behind the natural air drying;
It is characterized in that:
(2), pulse electrodeposition prepares the Ni-Mo-P/Ni electrode
Adopt two electrode systems, the Ni substrate of handling well with step (1) is a working electrode, and the Ni plate is a counter electrode; Consisting of of Ni-Mo-P plating bath: 20～60 g/L nickel salt aqueous solutions; 10～50 g/L molybdate aqueous solution; 10～60 g/L ortho phosphorous acid sodium water solutions, 20～150 g/L trisodium citrate aqueous solutions, 10～300 g/L sodium chloride aqueous solutions; The pH value of plating bath is 1～10, and bath temperature is 20～60 ℃; Pulse peak current density is 10～30A/dm
2, the pulse ON time is 0.1～10ms, and pulse turn-off time is 0.5～50ms, and electrodeposition time is 5～300s; Electroplate the end back and use deionized water rinsing,, make the Ni-Mo-P electrode behind the natural air drying to remove residual plating bath.
2. according to the described a kind of efficient Ni-Mo-P/Ni hydrogen-precipitating electrode preparation method of claim 1, it is characterized in that described nickel salt is one of them of single nickel salt, nickelous nitrate, nickelous chloride; Molybdate is one of them of Sodium orthomolybdate, ammonium molybdate.
3. according to the described a kind of efficient Ni-Mo-P/Ni hydrogen-precipitating electrode preparation method of claim 1, it is characterized in that concrete preparing method's step (2):
(2), pulse electrodeposition prepares the Ni-Mo-P/Ni electrode
Adopt two electrode systems, the Ni substrate of handling well with step (1) is a working electrode, and the Ni plate is a counter electrode; Consisting of of Ni-Mo-P plating bath: the 40g/L nickel sulfate solution, 30 g/L sodium molybdate aqueous solutions, 10 g/L ortho phosphorous acid sodium water solutions, 150 g/L trisodium citrate aqueous solutions, 200 g/L sodium chloride aqueous solutions, the pH value of plating bath is 8, bath temperature is 20 ℃; Pulse peak current density is 30A/dm
2, the pulse ON time is 1ms, and pulse turn-off time is 10ms, and electrodeposition time is 200s; Electroplate the end back and use deionized water rinsing,, make the Ni-Mo-P electrode behind the natural air drying to remove residual plating bath.
4. according to the described a kind of efficient Ni-Mo-P/Ni hydrogen-precipitating electrode preparation method of claim 1, it is characterized in that concrete preparing method's step (2):
(2), pulse electrodeposition prepares the Ni-Mo-P/Ni electrode
Adopt two electrode systems, the Ni substrate of handling well with step (1) is a working electrode, and the Ni plate is a counter electrode; Consisting of of Ni-Mo-P plating bath: the 20g/L nickel nitrate aqueous solution, 50 g/L sodium molybdate aqueous solutions, 60 g/L ortho phosphorous acid sodium water solutions, 150 g/L trisodium citrate aqueous solutions, 10 g/L sodium chloride aqueous solutions, the pH value of plating bath is 10, bath temperature is 60 ℃; Pulse peak current density is 30A/dm
2, the pulse ON time is 0.1ms, and pulse turn-off time is 0.5ms, and electrodeposition time is 5s; Electroplate the end back and use deionized water rinsing,, make the Ni-Mo-P electrode behind the natural air drying to remove residual plating bath.
5. according to the described a kind of efficient Ni-Mo-P/Ni hydrogen-precipitating electrode preparation method of claim 1, it is characterized in that concrete preparing method's step (2):
(2), pulse electrodeposition prepares the Ni-Mo-P/Ni electrode
Adopt two electrode systems, the Ni substrate of handling well with step (1) is a working electrode, and the Ni plate is a counter electrode; Consisting of of Ni-Mo-P plating bath: 60 g/L nickel chloride aqueous solutions, 10 g/L ammonium molybdate aqueous solutions, 30 g/L ortho phosphorous acid sodium water solutions, 20 g/L trisodium citrate aqueous solutions, 300 g/L sodium chloride aqueous solutions, the pH value of plating bath is 1, bath temperature is 40 ℃; Pulse peak current density is 10A/dm
2, the pulse ON time is 10ms, pulse turn-off time is 50ms, electrodeposition time 300s; Electroplate the end back and use deionized water rinsing,, make the Ni-Mo-P electrode behind the natural air drying to remove residual plating bath.
6. according to the described a kind of efficient Ni-Mo-P/Ni hydrogen-precipitating electrode preparation method of claim 1, it is characterized in that concrete preparing method's step (2):
(2), pulse electrodeposition prepares the Ni-Mo-P/Ni electrode
Adopt two electrode systems, the Ni substrate of handling well with step (1) is a working electrode, and the Ni plate is a counter electrode; Consisting of of Ni-Mo-P plating bath: 40 g/L nickel sulfate solutions, 30 g/L ammonium molybdate aqueous solutions, 30 g/L ortho phosphorous acid sodium water solutions, 70 g/L trisodium citrate aqueous solutions, 200 g/L sodium chloride aqueous solutions, the pH value of plating bath is 8, bath temperature is 20 ℃; Pulse peak current density is 20A/dm
2, the pulse ON time is 1ms, and pulse turn-off time is 10ms, and electrodeposition time is 200s; Electroplate the end back and use deionized water rinsing,, make the Ni-Mo-P electrode behind the natural air drying to remove residual plating bath.
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