CN103924260B - Compound hydrogen-precipitating electrode of a kind of three-dimensional foam Ni copper and cobalt and preparation method thereof - Google Patents
Compound hydrogen-precipitating electrode of a kind of three-dimensional foam Ni copper and cobalt and preparation method thereof Download PDFInfo
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Abstract
The present invention relates to one and can be used for electrocatalytic hydrogen evolution reaction in alkaline solution, the three-dimensional foam Ni copper of the base metal of load simultaneously hydrogen-precipitating electrode and hydrogen-precipitating electrode of cobalt and preparation method thereof, belong to materials science field and electro-catalysis hydrogen preparation field, technical problem to be solved has been to provide compound hydrogen-precipitating electrode of a kind of three-dimensional foam Ni copper and cobalt and preparation method thereof, it mainly adopts electrochemical surface composite deposite method, at three-dimensional foam nickel surface successively electro-coppering and cobalt, thereby make compound hydrogen-precipitating electrode, it is high that its electrode making has catalytic activity, nontoxic, can be stable at holding structure under alkali condition and chemism, and its preparation technology is simple, be applicable to large-scale production.
Description
Technical field
The present invention relates to one and can be used for electrocatalytic hydrogen evolution reaction in alkaline solution, the three-dimensional foam Ni copper of the base metal of load simultaneously hydrogen-precipitating electrode and hydrogen-precipitating electrode of cobalt and preparation method thereof, belong to materials science field and electro-catalysis hydrogen preparation field.
Background technology
What the mankind mainly utilized at present is the non-renewable fossil energy such as oil, coal, and due to the mankind's exhaustive exploitation, these fossil energies face exhausted danger already; And the use of fossil fuel causes serious environmental pollution to the mankind, such as greenhouse effects, acid rain and haze etc., the mankind's healthy and existence in serious threat. Hydrogen, because of advantages such as its source is abundant, cleanliness without any pollution, burning highly effectives, is considered to optimal energy carrier. Water electrolysis hydrogen production is one of important method likely realizing large-scale production hydrogen. In water electrolysis hydrogen production, the selection of electrode, the design of structure and preparation technology's optimization is the key of water electrolysis hydrogen production always, very important effect is played in its reduction, the raising of catalyst utilization and minimizing of electrolysis energy consumption to electrode cost, and can affect again electrolytic method large-scale industrial production simultaneously. The noble metal such as Pd and Pt is the metal electrode material with good electric catalytic hydrogen evolution activity, but because these noble metals are expensive, be difficult to widely apply in industrial production, therefore research and develop the novel cathode base metal material hydrogen-precipitating electrode that cheap, high activity and overpotential of hydrogen evolution are low extremely important.
Summary of the invention
The present invention overcomes the deficiency that prior art exists, and technical problem to be solved has been to provide compound hydrogen-precipitating electrode of a kind of three-dimensional foam Ni copper and cobalt and preparation method thereof. It mainly adopts electrochemical surface composite deposite method, at three-dimensional foam nickel surface successively electro-coppering and cobalt, it is high, nontoxic that the electrode making has catalytic activity, can be stable at holding structure under alkali condition and chemism, and its preparation technology is simple, is applicable to large-scale production.
For solving the problems of the technologies described above, the technical solution adopted in the present invention is: the compound hydrogen-precipitating electrode of a kind of three-dimensional foam Ni copper and cobalt, comprise: electrode, described electrode is to be carrier by three-dimensional foam nickel, copper and cobalt are carried metal, and be deposited on successively the surface of three-dimensional foam nickel by electrochemical method, and wherein metallic copper coating is interior, and metallic cobalt coating is outside.
Preferably, the purity of described carrier is 99.99% three-dimensional porous nickel foam, and porosity is 95%.
A preparation method for the compound hydrogen-precipitating electrode of three-dimensional foam Ni copper and cobalt, carries out according to following steps,
A, by three-dimensional foam nickel degreasing degreasing 1-2 minute in acetone, clean with ultra-pure water, be then placed on acidifying activation in the hydrochloric acid solution of 18wt.%, be finally placed on ultrasonic 4-7 minute in ultra-pure water;
B, three-dimensional foam nickel after treatment in step a is put in copper plating solution, taking copper sheet as anode, three-dimensional foam nickel is negative electrode, is 0.01-0.05A/cm in current density2Electric current under use multifunctional pulse electroplating power supply electro-deposition 500-700s;
C, by electrochemical deposition in step b the three-dimensional foam nickel of copper clean with ultra-pure water, and then in ultra-pure water ultrasonic 4-7 minute;
D, the three-dimensional foam nickel after ultrasonic in step c is put in cobalt plating solution, taking cobalt rod as anode, the three-dimensional foam nickel after copper facing is ultrasonic is negative electrode, is 0.01-0.05A/cm in current density2Electric current under use multifunctional pulse electroplating power supply electro-deposition 500-700s;
E, the three-dimensional foam nickel ultra-pure water that electrochemical deposition in steps d is crossed to copper and cobalt clean, then are placed in after the ultrasonic 4-7 of ultra-pure water minute;
Environment temperature in f, above-mentioned steps a, b, c, d, e is 10-30 DEG C, can obtain the compound hydrogen-precipitating electrode of three-dimensional foam Ni copper and cobalt.
Preferably, the copper plating solution in described step b or be pyrophosphate copper plating solution, or be alkaline cyanide-free copper plating solution, or be acid copper plating solution.
Preferably, the cobalt plating solution in described steps d or be sulfate cobalt plating solution, or be chloride system cobalt plating solution.
Preferably, described pyrophosphate copper plating solution or be copper pyrophosphate solution, or be one or both mixed liquor in copper pyrophosphate solution and potassium pyrophosphate solution, ammonium citrate solution; Described alkaline cyanide-free copper plating solution or be cupric sulfate pentahydrate solution, or be one or more mixed liquor in cupric sulfate pentahydrate solution and biuret solution, sodium hydroxide solution, glycerine; Described acid copper plating solution or be the mixed liquor of cupric sulfate pentahydrate and boric acid.
Preferably, described sulfate cobalt plating solution or be cobalt sulfate solution, or be one or both mixed liquor in cobalt sulfate solution and triethanolamine solution, ZCA additive; Described chloride system cobalt plating solution or be CoCL2 6H2O solution, or be the mixed liquor of CoCL2 6H2O and boric acid.
The present invention compared with prior art has following beneficial effect.
1, the three-dimensional foam Ni copper that prepared by the present invention and the hydrogen-precipitating electrode of cobalt, by using three-dimensional porous nickel foam to do carrier, effectively increased haptoreaction area.
2, the three-dimensional foam Ni copper that prepared by the present invention and the hydrogen-precipitating electrode of cobalt, by electrochemically depositing copper and cobalt on nickel foam, utilize its cooperative effect, greatly reduce the overpotential of hydrogen evolution of nickel foam, improved the performance of electrocatalytic hydrogen evolution and the stability of electrode.
3, in the present invention, base metal copper and cobalt and nickel foam are effectively combined, comparing other loads has precious metal element hydrogen-precipitating electrode, and raw material source is abundant, and low price, has reduced production cost greatly.
4, the present invention is by electrochemical method deposited copper thin layer and cobalt thin layer successively, and control, affected by environment little is stablized, is easy to this technical maturity.
5, the inventive method technique is simple, easy and simple to handle, is applicable to preparing on a large scale the compound hydrogen-precipitating electrode of high activity of three-dimensional foam Ni copper and cobalt.
Brief description of the drawings
Fig. 1 is the macrostate figure of the compound hydrogen-precipitating electrode of three-dimensional foam Ni copper and cobalt in the present invention.
Fig. 2 is that in the present invention, the compound hydrogen-precipitating electrode of three-dimensional foam Ni copper and cobalt amplifies the scanning electron microscope (SEM) photograph of 500 times.
Fig. 3 is that in the present invention, the compound hydrogen-precipitating electrode of three-dimensional foam Ni copper and cobalt amplifies the scanning electron microscope (SEM) photograph of 5000 times.
Fig. 4 is that the surface chemistry composition EDX of the compound hydrogen-precipitating electrode of three-dimensional foam Ni copper and cobalt in the present invention can spectrogram.
Fig. 5 is three-dimensional foam Ni copper and the compound hydrogen-precipitating electrode of cobalt and the XRD collection of illustrative plates comparison diagram of pure foam nickel electrode in the present invention.
Fig. 6 is three-dimensional foam Ni copper and the compound hydrogen-precipitating electrode of cobalt and the evolving hydrogen reaction cyclic voltammetric comparison diagram of pure foam nickel electrode in the present invention.
Detailed description of the invention
Below in conjunction with accompanying drawing, specific embodiments of the invention are described further.
The compound hydrogen-precipitating electrode of a kind of three-dimensional foam Ni copper and cobalt, comprise: electrode, it is characterized in that: described electrode is to be carrier by three-dimensional foam nickel, metallic copper and cobalt are carried metal, and by being electrochemically-deposited in the surface of three-dimensional foam nickel, described carrier is that purity is 99.99% three-dimensional porous nickel foam, and porosity is 95%.
As shown in Figure 1, the macrostate figure of the compound hydrogen-precipitating electrode of three-dimensional foam Ni copper and cobalt. Fig. 2 is low power scanning electron microscope (SEM) photograph, can see obvious three-dimensional framework structure. Fig. 3 is high power stereoscan photograph, can see that the compound hydrogen-precipitating electrode of three-dimensional foam nickel surface is owing to having deposited successively coarse that copper layer and cobalt layer become. Fig. 4 is the surface chemistry composition EDX energy spectrogram of the compound hydrogen-precipitating electrode of three-dimensional foam Ni copper and cobalt, and by finding out by spectrogram, the cobalt atom on electrode top layer approaches 99%, also has a small amount of copper atom to be detected.
Embodiment 1
A preparation method for the compound hydrogen-precipitating electrode of three-dimensional foam Ni copper and cobalt, carries out according to following steps,
A, by three-dimensional foam nickel degreasing degreasing 1 minute in acetone, clean with ultra-pure water, be then placed on acidifying activation in the hydrochloric acid solution of 18wt.%, be finally placed in ultra-pure water ultrasonic 4 minutes;
B, three-dimensional foam nickel after treatment in step a is put into copper pyrophosphate solution, or in copper pyrophosphate solution and potassium pyrophosphate solution, ammonium citrate solution in one or both mixed liquor, taking copper sheet as anode, three-dimensional foam nickel is negative electrode, is 0.01A/cm in current density2Electric current under use multifunctional pulse electroplating power supply electro-deposition 500s;
C, by electrochemical deposition in step b the three-dimensional foam nickel of copper clean with ultra-pure water, and then in ultra-pure water ultrasonic 4 minutes;
D, the three-dimensional foam nickel after ultrasonic in step c is put into cobalt sulfate solution, or in cobalt sulfate solution and triethanolamine solution, ZCA additive in one or both mixed liquor, taking cobalt rod as anode, three-dimensional foam nickel after copper facing is ultrasonic is negative electrode, is 0.05A/cm in current density2Electric current under use multifunctional pulse electroplating power supply electro-deposition 500s;
E, the three-dimensional foam nickel ultra-pure water that electrochemical deposition in steps d is crossed to copper and cobalt clean, then are placed in ultra-pure water after ultrasonic 4 minutes;
Environment temperature in f, above-mentioned steps a, b, c, d, e is 10 DEG C, can obtain the compound hydrogen-precipitating electrode of three-dimensional foam Ni copper and cobalt.
Embodiment 2
A preparation method for the compound hydrogen-precipitating electrode of three-dimensional foam Ni copper and cobalt, carries out according to following steps,
A, by three-dimensional foam nickel degreasing degreasing 1 minute in acetone, clean with ultra-pure water, be then placed on acidifying activation in the hydrochloric acid solution of 18wt.%, be finally placed in ultra-pure water ultrasonic 5 minutes;
B, three-dimensional foam nickel after treatment in step a is put into cupric sulfate pentahydrate solution, or in cupric sulfate pentahydrate solution and biuret solution, sodium hydroxide solution, glycerine in one or more mixed liquor, taking copper sheet as anode, three-dimensional foam nickel is negative electrode, is 0.03A/cm in current density2Electric current under use multifunctional pulse electroplating power supply electro-deposition 600s;
C, by electrochemical deposition in step b the three-dimensional foam nickel of copper clean with ultra-pure water, and then in ultra-pure water ultrasonic 5 minutes;
D, the three-dimensional foam nickel after ultrasonic in step c is put in the solution of cobalt sulfate and triethanolamine, taking cobalt rod as anode, the three-dimensional foam nickel after copper facing is ultrasonic is negative electrode, is 0.03A/cm in current density2Electric current under use multifunctional pulse electroplating power supply electro-deposition 600s;
E, the three-dimensional foam nickel ultra-pure water that electrochemical deposition in steps d is crossed to copper and cobalt clean, then are placed in ultra-pure water after ultrasonic 5 minutes;
Environment temperature in f, above-mentioned steps a, b, c, d, e is 20 DEG C, can obtain the compound hydrogen-precipitating electrode of three-dimensional foam Ni copper and cobalt.
Embodiment 3
A preparation method for the compound hydrogen-precipitating electrode of three-dimensional foam Ni copper and cobalt, carries out according to following steps,
A, by three-dimensional foam nickel degreasing degreasing 1 minute in acetone, clean with ultra-pure water, be then placed on acidifying activation in the hydrochloric acid solution of 18wt.%, be finally placed in ultra-pure water ultrasonic 7 minutes;
B, three-dimensional foam nickel after treatment in step a is put in the mixed liquor of cupric sulfate pentahydrate and boric acid, taking copper sheet as anode, three-dimensional foam nickel is negative electrode, is 0.05A/cm in current density2Electric current under use multifunctional pulse electroplating power supply electro-deposition 700s;
C, by electrochemical deposition in step b the three-dimensional foam nickel of copper clean with ultra-pure water, and then in ultra-pure water ultrasonic 7 minutes;
D, the three-dimensional foam nickel after ultrasonic in step c is put in CoCL2 6H2O and boric acid mixed solution, taking cobalt rod as anode, the three-dimensional foam nickel after copper facing is ultrasonic is negative electrode, is 0.01A/cm in current density2Electric current under use multifunctional pulse electroplating power supply electro-deposition 700s;
E, the three-dimensional foam nickel ultra-pure water that electrochemical deposition in steps d is crossed to copper and cobalt clean, then are placed in ultra-pure water after ultrasonic 7 minutes;
Environment temperature in f, above-mentioned steps a, b, c, d, e is 30 DEG C, can obtain the compound hydrogen-precipitating electrode of three-dimensional foam Ni copper and cobalt.
As shown in Figure 5, the XRD crystal structure figure contrast of the compound hydrogen-precipitating electrode of pure foam nickel and three-dimensional foam Ni copper and cobalt, can see that surperficial cobalt is face-centred cubic structure, its diffraction maximum almost overlaps with the diffraction maximum of matrix nickel, can detect faint copper diffraction maximum simultaneously. The cyclic voltammetric liberation of hydrogen curve of the compound hydrogen-precipitating electrode that Fig. 6 has provided respectively pure foam nickel and three-dimensional foam Ni copper and cobalt in 1.0M potassium hydroxide solution, sweep speed is 50mVs-1, the compound hydrogen-precipitating electrode of three-dimensional foam Ni copper and cobalt shows obviously high electrocatalytic hydrogen evolution activity.
In sum, three-dimensional foam Ni copper prepared by the present invention and the hydrogen-precipitating electrode of cobalt, by using three-dimensional porous nickel foam to do carrier, effectively increased haptoreaction area; By electrochemically depositing copper layer and cobalt layer successively on nickel foam, utilize its cooperative effect, greatly reduce the overpotential of hydrogen evolution of nickel foam, improve the stability of its electrocatalytic hydrogen evolution performance and electrode, by base metal copper and cobalt and nickel foam are effectively combined, comparing other loads has the hydrogen-precipitating electrode of precious metal element simultaneously, and raw material source is abundant, low price, greatly reduces production cost.
By reference to the accompanying drawings embodiments of the invention are described in detail above; but the present invention is not limited to above-described embodiment; in the ken possessing those of ordinary skill in the art; can also under the prerequisite that does not depart from aim of the present invention, make obtaining various variations, also should be considered as protection scope of the present invention.
Claims (7)
1. the compound hydrogen-precipitating electrode of a three-dimensional foam Ni copper and cobalt, comprise: electrode, it is characterized in that: described electrode is to be carrier by three-dimensional foam nickel, copper and cobalt are carried metal, and be deposited on successively the surface of three-dimensional foam nickel by electrochemical method, wherein metallic copper coating is interior, and metallic cobalt coating outside.
2. the compound hydrogen-precipitating electrode of a kind of three-dimensional foam Ni copper as claimed in claim 1 and cobalt, is characterized in that: the purity of described carrier is 99.99% three-dimensional porous nickel foam, and porosity is 95%.
3. the preparation method of the compound hydrogen-precipitating electrode of a kind of three-dimensional foam Ni copper as claimed in claim 1 and cobalt, is characterized in that: carries out according to following steps,
A, by three-dimensional foam nickel degreasing degreasing 1-2 minute in acetone, clean with ultra-pure water, be then placed on acidifying activation in the hydrochloric acid solution of 18wt.%, be finally placed on ultrasonic 4-7 minute in ultra-pure water;
B, three-dimensional foam nickel after treatment in step a is put in copper plating solution, taking copper sheet as anode, three-dimensional foam nickel is negative electrode, is 0.01-0.05A/cm in current density2Electric current under use multifunctional pulse electroplating power supply electro-deposition 500-700s;
C, by electrochemical deposition in step b the three-dimensional foam nickel of copper clean with ultra-pure water, and then in ultra-pure water ultrasonic 4-7 minute;
D, the three-dimensional foam nickel after ultrasonic in step c is put in cobalt plating solution, taking cobalt rod as anode, the three-dimensional foam nickel after copper facing is ultrasonic is negative electrode, is 0.01-0.05A/cm in current density2Electric current under use multifunctional pulse electroplating power supply electro-deposition 500-700s;
E, the three-dimensional foam nickel ultra-pure water that electrochemical deposition in steps d is crossed to copper and cobalt clean, then are placed in after the ultrasonic 4-7 of ultra-pure water minute;
Environment temperature in f, above-mentioned steps a, b, c, d, e is 10-30 DEG C, can obtain the compound hydrogen-precipitating electrode of three-dimensional foam Ni copper and cobalt.
4. the preparation method of the compound hydrogen-precipitating electrode of a kind of three-dimensional foam Ni copper as claimed in claim 3 and cobalt, it is characterized in that: the copper plating solution in described step b or for pyrophosphate copper plating solution, or be alkaline cyanide-free copper plating solution, or be acid copper plating solution.
5. the preparation method of the compound hydrogen-precipitating electrode of a kind of three-dimensional foam Ni copper as claimed in claim 3 and cobalt, is characterized in that: the cobalt plating solution in described steps d or for sulfate cobalt plating solution, or be chloride system cobalt plating solution.
6. the preparation method of the compound hydrogen-precipitating electrode of a kind of three-dimensional foam Ni copper as claimed in claim 4 and cobalt, it is characterized in that: described pyrophosphate copper plating solution or for copper pyrophosphate solution, or be one or both mixed liquor in copper pyrophosphate solution and potassium pyrophosphate solution, ammonium citrate solution; Described alkaline cyanide-free copper plating solution or be cupric sulfate pentahydrate solution, or be one or more mixed liquor in cupric sulfate pentahydrate solution and biuret solution, sodium hydroxide solution, glycerine; Described acid copper plating solution or be the mixed liquor of cupric sulfate pentahydrate and boric acid.
7. the preparation method of the compound hydrogen-precipitating electrode of a kind of three-dimensional foam Ni copper as claimed in claim 5 and cobalt, it is characterized in that: described sulfate cobalt plating solution or for cobalt sulfate solution, or be one or both mixed liquor in cobalt sulfate solution and triethanolamine solution, ZCA additive; Described chloride system cobalt plating solution or be CoCL2 6H2O solution, or be the mixed liquor of CoCL2 6H2O and boric acid.
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