CN102899681A - Porous nickel composite electrode, electroplating solution and preparation method of porous nickel composite electrode - Google Patents
Porous nickel composite electrode, electroplating solution and preparation method of porous nickel composite electrode Download PDFInfo
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- CN102899681A CN102899681A CN2012104215412A CN201210421541A CN102899681A CN 102899681 A CN102899681 A CN 102899681A CN 2012104215412 A CN2012104215412 A CN 2012104215412A CN 201210421541 A CN201210421541 A CN 201210421541A CN 102899681 A CN102899681 A CN 102899681A
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Abstract
The invention relates to a porous nickel composite electrode, which comprises a substrate nickel plate, and LaNi5 particles adhered to the substrate nickel plate. An electroplating solution for preparing the porous nickel composite electrode comprises the following components: NiSO4 . 6H2O: 300 g . L<-1>, NiCl2 . 6H2O: 50g . L<-1>, H3BO3: 40g . L<-1>, aluminum powder: 30g . L<-1> and LaNi5 particles: 25g . L<-1>, and the pH is 4.0 to 5.0. A hydrogen storage alloy LaNi5 and Al particle capsules are embedded into a plating layer on a substrate Ni by one-step composite electrodeposition to obtain an Ni/(LaNi5 + Al) precursor, and then aluminum in the plating layer is dissolved by an alkali dissolving method. The porous nickel composite electrode prepared by the invention has the advantages of larger specific surface area, lower hydrogen evolution overpotential, excellent hydrogen evolution electrocatalytic properties, and excellent outage resistance and corrosion resistance, i.e., excellent stability property.
Description
[technical field]
The present invention relates to a kind of nickel porous combined electrode, for the preparation of the electroplate liquid of this nickel porous combined electrode, and the preparation method of this nickel porous combined electrode.
[background technology]
Water electrolysis is one of important technology of preparation high-purity hydrogen, as long as provide certain forms a certain amount of electric energy, then can make water decomposition.Provide electric energy to make efficient that water decomposition makes hydrogen generally 75%～85%, its technological process is simple, pollution-free, but consumes power is large, so that its application is subject to certain restrictions.In order to reduce the hydrogen manufacturing cost, must seek more effective hydrogen evolution electrode material and reduce overpotential of hydrogen evolution, to reduce unit of electrical energy consumption.Nickel has moderate absorption hydrogen bond energy because of its special not paired d electron structure, so its electrocatalytic hydrogen evolution better performances, and price is lower, aboundresources.Just because of this, the alloys such as nickel and nickel molybdenum are the Electrocatalytic Activity for Hydrogen Evolution Reaction materials of commonly using, and industrially make Raney's nickel or netted nickelalloy is the hydrogen-precipitating electrode of commonly using, and this class electrode electro catalytic activity is higher, porosity is high, specific surface area is large, and evolving hydrogen reaction speed is fast.But in electrolytic process, because gap electrolysis or stop outage (discontinuous electrolysis) particularly stopped more than two weeks of electrolysis, electrode is because atmospheric oxidation and corrosion, and nickel and alloy electrode electro catalytic activity thereof are decayed very soon, and electrode stability is bad.In a word, the anti-outage of existing electrode, short-circuit capacity are poor, and under not electrolysis state, electrode is oxidized and corrosion easily.
[summary of the invention]
One of technical problem to be solved by this invention is to provide a kind of nickel porous combined electrode, has higher specific surface area, lower overpotential of hydrogen evolution and higher anti-outage stability.
The present invention is what one of to solve the problems of the technologies described above by the following technical programs: a kind of nickel porous combined electrode, contain matrix nickel plate, and be attached to the LaNi on the described matrix nickel plate
5Particle, described LaNi
5The median size of particle is 20 μ m.
It is a kind of for the preparation of described nickel porous combined electrode electroplate liquid that two of technical problem to be solved by this invention is to provide, compound Electrocatalytic Activity for Hydrogen Evolution Reaction and the stability with excellence of made nickel porous.
The present invention be solve the problems of the technologies described above by the following technical programs two: a kind of for the preparation of described nickel porous combined electrode electroplate liquid, comprise NiSO
46H
2O 300gL
-1, NiCl
26H
2O 50gL
-1, H
3BO
340gL
-1, aluminium powder 30gL
-1, LaNi
5Particle 25gL
-1, and the pH of described electroplate liquid is 4.0～5.0; The median size of described aluminium powder is 10 μ m, described LaNi
5The particle median size is 20 μ m.
Further, the temperature of described electroplate liquid is 45 ℃.
Further, the current density 40～70mAcm of described electroplate liquid
-2
Further, the negative electrode of described electroplate liquid is the latten(-tin) of 1.7cm * 1.7cm of being coated with 10 μ m nickel coatings * 0.3cm, and anode is the pure nickel plate of 6cm * 9cm * 0.5cm.
Three of technical problem to be solved by this invention is to provide a kind of preparation method of described nickel porous combined electrode, form nickel composite deposite at Ni substrate through epitaxy, there is not the interface to exist, coating and basal body binding force are good, the nickel porous combined electrode that makes had both had larger specific surface area, lower overpotential of hydrogen evolution, therefore, have excellent Electrocatalytic Activity for Hydrogen Evolution Reaction and stability.
The present invention be solve the problems of the technologies described above by the following technical programs three: a kind of preparation method of described nickel porous combined electrode may further comprise the steps:
(1) solia particle pre-treatment: be that aluminium powder, the median size of 10 μ m is the LaNi of 20 μ m with median size
5Particle is oil removing in 8.0 the weak base, filtration respectively at the pH value, then with a large amount of distilled water flushings, again with tensio-active agent processing, filtration, distilled water flushing, oven dry;
(2) by following formulated electroplate liquid: NiSO
46H
2O 300gL
-1, NiCl
26H
2O 50gL
-1, H
3BO
340gL
-1, aluminium powder 30gL
-1, LaNi
5Particle 25gL
-1, this plating bath pH is 4.0～5.0, the distilled water preparation;
(3) electroplate: the latten(-tin) with the 1.7cm * 1.7cm that is coated with 10 μ m nickel coatings * 0.3cm is negative electrode, and the pure nickel plate of 6cm * 9cm * 0.5cm is anode, with negative electrode place plating bath parallel with anode, in current density 40～70mAcm
-2, electroplate 20min under the temperature 45 C, obtain Ni/ (Al+LaNi
5) precursor;
(4) preparation electrode: with the Ni/ (Al+LaNi that obtains in (3)
5) precursor is positioned over temperature 60 C, 6molL
-1NaOH solution in to emerging to remove aluminium without bubble, then take out, clean with distilled water, dry up, obtain the nickel porous combined electrode.
Further, the weak base in the described step (1) is ammoniacal liquor.
Further, the tensio-active agent in the described step (1) is the polyoxyethylene glycol of 1g/L.
Beneficial effect of the present invention is: the present invention goes on foot composite electrodeposition with hydrogen storage alloy LaNi by one first on matrix nickel
5Be embedded into Al particle capsule and obtained Ni/ (LaNi in the coating
5Then+Al) composite deposite adopts alkali solution technique that the al dissolution in the coating is fallen, and makes the compound Ni/LaNi of porous
5Electrode.Because electronickelling composite deposite on matrix nickel belongs to epitaxy coating, do not have the interface between composite deposite and matrix to exist, so coating and basal body binding force are good, the compound Ni/LaNi of the porous that makes
5Electrode had both had larger specific surface area, lower overpotential of hydrogen evolution, namely had excellent Electrocatalytic Property for Hydrogen Evolution, had again good anti-outage, corrosion resistance, namely had good stability.
[description of drawings]
The invention will be further described in conjunction with the embodiments with reference to the accompanying drawings.
Fig. 1 a is Ni/Al precursor SEM figure among the present invention;
Fig. 1 b is porous nickel electrode SEM figure among the present invention;
Fig. 1 c is Ni/Al+LaNi among the present invention
5Precursor SEM figure;
Fig. 1 d is the compound Ni/LaNi of porous among the present invention
5Electrode SEM figure;
Fig. 2 is porous nickel electrode and the compound Ni/LaNi of porous among the present invention
5Potentiostatic deposition electric current and the time curve of electrode;
Fig. 3 is porous nickel electrode and the compound Ni/LaNi of porous among the present invention
5The constant potential of electrode is interrupted Faradaic current and time curve;
Fig. 4 is the compound Ni/LaNi of porous among the present invention
5Potentiostatic deposition electric current and the time curve of electrode after three weeks of cutting off the power supply.
[embodiment]
A kind of nickel porous combined electrode contains matrix nickel plate, and is attached to the LaNi on the described matrix nickel plate
5Particle, described LaNi
5The median size of particle is 20 μ m.
A kind of for the preparation of described nickel porous combined electrode electroplate liquid, comprise NiSO
46H
2O 300gL
-1, NiCl
26H
2O 50gL
-1, H
3BO
340gL
-1, aluminium powder 30gL
-1, LaNi
5Particle 25gL
-1, and the pH of described electroplate liquid is 4.0～5.0; The median size of described aluminium powder is 10 μ m, described LaNi
5The particle median size is 20 μ m; The temperature of described electroplate liquid is 45 ℃; Current density 40～the 70mAcm of described electroplate liquid
-2The negative electrode of described electroplate liquid is the latten(-tin) of 1.7cm * 1.7cm of being coated with 10 μ m nickel coatings * 0.3cm, and anode is the pure nickel plate of 6cm * 9cm * 0.5cm.
A kind of described nickel porous combined electrode is the compound Ni/LaNi of porous
5The preparation method of electrode may further comprise the steps:
(1) solia particle pre-treatment: be that aluminium powder, the median size of 10 μ m is the LaNi of 20 μ m with median size
5Particle is oil removing in 8.0 the weak base, filtration respectively at the pH value, then with a large amount of distilled water flushings, again with tensio-active agent processing, filtration, distilled water flushing, oven dry; Described weak base is ammoniacal liquor; Described tensio-active agent is the polyoxyethylene glycol of 1g/L.
(2) by following formulated electroplate liquid: NiSO
46H
2O 300gL
-1, NiCl
26H
2O 50gL
-1, H
3BO
340gL
-1, aluminium powder 30gL
-1, LaNi
5Particle 25gL
-1, this plating bath pH is 4.0～5.0, the distilled water preparation;
(3) electroplate: the latten(-tin) with the 1.7cm * 1.7cm that is coated with 10 μ m nickel coatings * 0.3cm is negative electrode, and the pure nickel plate of 6cm * 9cm * 0.5cm is anode, with negative electrode place plating bath parallel with anode, in current density 40～70mAcm
-2, electroplate 20min under the temperature 45 C, obtain Ni/ (Al+LaNi
5) precursor;
(4) preparation electrode: with the Ni/ (Al+LaNi that obtains in (3)
5) precursor is positioned over temperature 60 C, 6molL
-1NaOH solution in to emerging to remove aluminium without bubble, then take out, clean with distilled water, dry up, obtaining the nickel porous combined electrode is the compound Ni/LaNi of porous
5Electrode.
Following content provides exemplary embodiment of the present invention, and these embodiment only are exemplary, and is not used in restriction scope of the present invention as herein described, and these embodiment only are used for illustrating implementation method of the present invention:
Embodiment one
The preparation method of described nickel porous combined electrode may further comprise the steps:
(1) solia particle pre-treatment: be that aluminium powder, the median size of 10 μ m is the LaNi of 20 μ m with median size
5Particle is oil removing in 8.0 the ammoniacal liquor, filtration respectively at the pH value, then with a large amount of distilled water flushings, uses polyoxyethylene glycol processing, filtration, distilled water flushing, the oven dry of 1g/L again.
(2) by following formulated electroplate liquid: NiSO
46H
2O 300gL
-1, NiCl
26H
2O 50gL
-1, H
3BO
340gL
-1, aluminium powder 30gL
-1, LaNi
5Particle 25gL
-1, this plating bath pH is 4.0, the distilled water preparation;
(3) electroplate: the latten(-tin) with the 1.7cm * 1.7cm that is coated with 10 μ m nickel coatings * 0.3cm is negative electrode, and the pure nickel plate of 6cm * 9cm * 0.5cm is anode, with negative electrode place plating bath parallel with anode, in current density 40mAcm
-2, electroplate 20min under the temperature 45 C, obtain Ni/ (Al+LaNi
5) precursor;
(4) preparation electrode: with the Ni/ (Al+LaNi that obtains in (3)
5) precursor is positioned over temperature 60 C, 6molL
-1NaOH solution in to emerging to remove aluminium without bubble, then take out, clean with distilled water, dry up, obtaining the nickel porous combined electrode is the compound Ni/LaNi of porous
5Electrode.
Embodiment two
This part is with embodiment one difference:
(2) by following formulated electroplate liquid: this plating bath pH is 5.0;
(3) electroplate: current density 70mAcm
-2
Embodiment three
This part is with embodiment one difference:
(2) by following formulated electroplate liquid: this plating bath pH is 4.5;
(3) electroplate: current density 50mAcm
-2
Embodiment four
A kind of preparation of porous nickel electrode may further comprise the steps:
(1) solia particle pre-treatment: the aluminium powder that with median size is 10 μ m is oil removing in 8.0 the ammoniacal liquor, filtration in the pH value, then with a large amount of distilled water flushings, uses polyoxyethylene glycol processing, filtration, distilled water flushing, the oven dry of 1g/L again.
(2) by following formulated electroplate liquid: NiSO
46H
2O 300gL
-1, NiCl
26H
2O 50gL
-1, H
3BO
340gL
-1, aluminium powder 30gL
-1, this plating bath pH is 4.0, the distilled water preparation;
(3) electroplate: the latten(-tin) with the 1.7cm * 1.7cm that is coated with 10 μ m nickel coatings * 0.3cm is negative electrode, and the pure nickel plate of 6cm * 9cm * 0.5cm is anode, with negative electrode place plating bath parallel with anode, in current density 40mAcm
-2, electroplate 20min under the temperature 45 C, obtain the Ni/Al precursor;
(4) preparation porous nickel electrode: the nickel porous precursor that obtains in (3) is positioned over temperature 60 C, 6molL
-1NaOH solution in to emerging to remove aluminium without bubble, then take out, clean with distilled water, dry up, obtain porous nickel electrode.
The Ni/Al+LaNi that embodiment one is made
5Precursor, the compound Ni/LaNi of porous
5Electrode, the Ni/Al precursor that embodiment four makes, porous nickel electrode carry out respectively SEM and characterize, and (shown in Fig. 1 a, Fig. 1 b, Fig. 1 c and Fig. 1 d), by Fig. 1 b and Fig. 1 d as seen, the compound Ni/LaNi of porous nickel electrode and porous
5Electrode is vesicular structure, and the compound Ni/LaNi of product porous of the present invention
5The specific surface area of electrode is 398.8, and the specific surface area of the porous nickel electrode for preparing under the same terms only is 39.8, as seen, and the compound Ni/LaNi of product porous of the present invention
5Electrode has larger specific surface area.
As shown in Figure 2, wherein curve a is the potentiostatic deposition electric current of porous nickel electrode and the relation curve of time, and curve b is the compound Ni/LaNi of porous of the present invention
5The potentiostatic deposition electric current of electrode and the relation curve of time, as shown in Figure 2, under same potential, the compound Ni/LaNi of porous of the present invention
5Electrode is that the electric current of curve b is larger, illustrates that resistance is less, impedance is little, shows the compound Ni/LaNi of porous
5The electro catalytic activity of electrode is high.In addition, along with the prolongation of time, curve b keeps horizontal linear always, and the compound Ni/LaNi of porous of the present invention is described
5The electrocatalysis good stability of electrode is difficult for along with the prolongation of time is fluctuateed.
Curve a among Fig. 3 is that the constant potential of porous nickel electrode is interrupted Faradaic current and the relation curve of time, and curve b is the compound Ni/LaNi of porous of the present invention
5The constant potential of electrode is interrupted Faradaic current and the relation curve of time, as seen from Figure 3, and again energising after repeatedly being interrupted outage, the compound Ni/LaNi of porous
5The electric current of electrode remains unchanged substantially, does not descend, and proves the compound Ni/LaNi of porous of the present invention
5The anti-outage excellent in stability of electrode, the difficult fluctuation.
Can be seen by Fig. 4, after long-time outage namely cut off the power supply for three weeks, the compound Ni/LaNi of porous
5It is high-order that the electric current of electrode also can keep, and further specifies the compound Ni/LaNi of porous of the present invention
5The anti-outage excellent in stability of electrode.
In sum, the present invention goes on foot composite electrodeposition with hydrogen storage alloy LaNi by one first on matrix nickel
5Be embedded into Al particle capsule and obtained Ni/ (LaNi in the coating
5Then+Al) composite deposite adopts alkali solution technique that the al dissolution in the coating is fallen, and makes the compound Ni/LaNi of porous
5Electrode.Because electronickelling composite deposite on matrix nickel belongs to epitaxy coating, do not have the interface between composite deposite and matrix to exist, so coating and basal body binding force are good, the compound Ni/LaNi of the porous that makes
5Electrode had both had larger specific surface area, lower overpotential of hydrogen evolution, namely had excellent Electrocatalytic Property for Hydrogen Evolution, had again good anti-outage, corrosion resistance, namely had good stability.
Claims (8)
1. a nickel porous combined electrode is characterized in that: contain matrix nickel plate, and be attached to the LaNi on the described matrix nickel plate
5Particle, described LaNi
5The median size of particle is 20 μ m.
2. one kind for the preparation of nickel porous combined electrode electroplate liquid claimed in claim 1, it is characterized in that: comprise NiSO
46H
2O 300gL
-1, NiCl
26H
2O 50gL
-1, H
3BO
340gL
-1, aluminium powder 30gL
-1, LaNi
5Particle 25gL
-1, and the pH of described electroplate liquid is 4.0～5.0; The median size of described aluminium powder is 10 μ m, described LaNi
5The particle median size is 20 μ m.
3. as claimed in claim 2 for the preparation of nickel porous combined electrode electroplate liquid, it is characterized in that: the temperature of described electroplate liquid is 45 ℃.
4. as claimed in claim 2 for the preparation of nickel porous combined electrode electroplate liquid, it is characterized in that: the current density 40～70mAcm of described electroplate liquid
-2
5. as claimed in claim 2 for the preparation of nickel porous combined electrode electroplate liquid, it is characterized in that: the negative electrode of described electroplate liquid is the latten(-tin) of 1.7cm * 1.7cm of being coated with 10 μ m nickel coatings * 0.3cm, and anode is the pure nickel plate of 6cm * 9cm * 0.5cm.
6. the preparation method of a nickel porous combined electrode as claimed in claim 1 is characterized in that: may further comprise the steps:
(1) solia particle pre-treatment: be that aluminium powder, the median size of 10 μ m is the LaNi of 20 μ m with median size
5Particle is oil removing in 8.0 the weak base, filtration respectively at the pH value, then with a large amount of distilled water flushings, again with tensio-active agent processing, filtration, distilled water flushing, oven dry;
(2) by following formulated electroplate liquid: NiSO
46H
2O 300gL
-1, NiCl
26H
2O 50gL
-1, H
3BO
340gL
-1, aluminium powder 30gL
-1, LaNi
5Particle 25gL
-1, this plating bath pH is 4.0～5.0, the distilled water preparation;
(3) electroplate: the latten(-tin) with the 1.7cm * 1.7cm that is coated with 10 μ m nickel coatings * 0.3cm is negative electrode, and the pure nickel plate of 6cm * 9cm * 0.5cm is anode, with negative electrode place plating bath parallel with anode, in current density 40～70mAcm
-2, electroplate 20min under the temperature 45 C, obtain Ni/ (Al+LaNi
5) precursor;
(4) preparation electrode: with the Ni/ (Al+LaNi that obtains in (3)
5) precursor is positioned over temperature 60 C, 6molL
-1NaOH solution in to emerging to remove aluminium without bubble, then take out, clean with distilled water, dry up, obtain the nickel porous combined electrode.
7. the preparation method of nickel porous combined electrode as claimed in claim 6, it is characterized in that: the weak base in the described step (1) is ammoniacal liquor.
8. the preparation method of nickel porous combined electrode as claimed in claim 6, it is characterized in that: the tensio-active agent in the described step (1) is the polyoxyethylene glycol of 1g/L.
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| WO2015003567A1 (en) * | 2013-07-12 | 2015-01-15 | City University Of Hong Kong | Porous framework and method for its manufacture |
| CN104372374A (en) * | 2014-07-21 | 2015-02-25 | 胡松 | Cathode catalyst and cathode structure of membrane electrode electrolysis ozone generator |
| US9840789B2 (en) | 2014-01-20 | 2017-12-12 | City University Of Hong Kong | Etching in the presence of alternating voltage profile and resulting porous structure |
| CN108048870A (en) * | 2017-12-20 | 2018-05-18 | 福州大学 | A kind of Ni-based active electrode material of embedded ruthenium Si composite oxide and preparation method thereof |
| CN108048895A (en) * | 2017-12-20 | 2018-05-18 | 福州大学 | A kind of Ni-based active electrode material of embedded ruthenium zirconium mixed oxide and preparation method thereof |
| CN108048869A (en) * | 2017-12-20 | 2018-05-18 | 福州大学 | A kind of Ni-based active electrode material of embedded ruthenium hafnium composite oxides and preparation method thereof |
| CN108855098A (en) * | 2018-05-24 | 2018-11-23 | 天津工业大学 | A kind of multistage pore canal nickel alumin(i)um alloy film and preparation method thereof with electrocatalysis characteristic |
| EP3460102A1 (en) * | 2017-09-21 | 2019-03-27 | Hymeth ApS | Method of producing an electrocatalyst |
| CN110504457A (en) * | 2019-08-21 | 2019-11-26 | 中国华能集团清洁能源技术研究院有限公司 | A kind of nickel base electrode antiseptic property optimization method |
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| US9840789B2 (en) | 2014-01-20 | 2017-12-12 | City University Of Hong Kong | Etching in the presence of alternating voltage profile and resulting porous structure |
| CN104372374A (en) * | 2014-07-21 | 2015-02-25 | 胡松 | Cathode catalyst and cathode structure of membrane electrode electrolysis ozone generator |
| EP3460102A1 (en) * | 2017-09-21 | 2019-03-27 | Hymeth ApS | Method of producing an electrocatalyst |
| WO2019057763A1 (en) * | 2017-09-21 | 2019-03-28 | Hymeth Aps | Method of producing an electrocatalyst |
| CN108048895A (en) * | 2017-12-20 | 2018-05-18 | 福州大学 | A kind of Ni-based active electrode material of embedded ruthenium zirconium mixed oxide and preparation method thereof |
| CN108048869A (en) * | 2017-12-20 | 2018-05-18 | 福州大学 | A kind of Ni-based active electrode material of embedded ruthenium hafnium composite oxides and preparation method thereof |
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| CN110504457B (en) * | 2019-08-21 | 2022-04-26 | 中国华能集团清洁能源技术研究院有限公司 | Method for optimizing corrosion resistance of nickel-based electrode |
| CN113249749A (en) * | 2021-05-10 | 2021-08-13 | 张家港智电芳华蓄电研究所有限公司 | Electrochemical hydrogen evolution electrode and preparation method thereof |
| CN113249749B (en) * | 2021-05-10 | 2022-11-22 | 张家港智电芳华蓄电研究所有限公司 | Electrochemical hydrogen evolution electrode and preparation method thereof |
| CN115074792A (en) * | 2022-07-07 | 2022-09-20 | 中国计量大学 | Preparation method of cobalt-based alloy film with special structure and product |
| CN115074792B (en) * | 2022-07-07 | 2024-01-16 | 中国计量大学 | Preparation method of cobalt-based alloy film with special structure and product |
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