CN114318398A - Water electrolysis hydrogen production electrode and preparation method thereof - Google Patents
Water electrolysis hydrogen production electrode and preparation method thereof Download PDFInfo
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- CN114318398A CN114318398A CN202210063908.1A CN202210063908A CN114318398A CN 114318398 A CN114318398 A CN 114318398A CN 202210063908 A CN202210063908 A CN 202210063908A CN 114318398 A CN114318398 A CN 114318398A
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- 229910052739 hydrogen Inorganic materials 0.000 title claims abstract description 28
- 239000001257 hydrogen Substances 0.000 title claims abstract description 28
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 title claims abstract description 28
- UFHFLCQGNIYNRP-UHFFFAOYSA-N Hydrogen Chemical compound [H][H] UFHFLCQGNIYNRP-UHFFFAOYSA-N 0.000 title claims abstract description 27
- 238000004519 manufacturing process Methods 0.000 title claims abstract description 16
- 238000002360 preparation method Methods 0.000 title claims abstract description 10
- 238000005868 electrolysis reaction Methods 0.000 title claims description 11
- 239000000956 alloy Substances 0.000 claims abstract description 13
- 229910045601 alloy Inorganic materials 0.000 claims abstract description 10
- 238000000866 electrolytic etching Methods 0.000 claims abstract description 6
- PXHVJJICTQNCMI-UHFFFAOYSA-N Nickel Chemical compound [Ni] PXHVJJICTQNCMI-UHFFFAOYSA-N 0.000 claims description 34
- 238000009713 electroplating Methods 0.000 claims description 27
- 239000000758 substrate Substances 0.000 claims description 21
- 229910052759 nickel Inorganic materials 0.000 claims description 15
- XEEYBQQBJWHFJM-UHFFFAOYSA-N Iron Chemical compound [Fe] XEEYBQQBJWHFJM-UHFFFAOYSA-N 0.000 claims description 14
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 claims description 13
- RYGMFSIKBFXOCR-UHFFFAOYSA-N Copper Chemical compound [Cu] RYGMFSIKBFXOCR-UHFFFAOYSA-N 0.000 claims description 13
- 229910052802 copper Inorganic materials 0.000 claims description 13
- 239000010949 copper Substances 0.000 claims description 13
- 238000000034 method Methods 0.000 claims description 10
- 229910002804 graphite Inorganic materials 0.000 claims description 7
- 239000010439 graphite Substances 0.000 claims description 7
- 229910052742 iron Inorganic materials 0.000 claims description 7
- 239000001509 sodium citrate Substances 0.000 claims description 5
- 229910021205 NaH2PO2 Inorganic materials 0.000 claims description 4
- 238000006243 chemical reaction Methods 0.000 claims description 3
- 229910052751 metal Inorganic materials 0.000 claims description 3
- 239000002184 metal Substances 0.000 claims description 3
- 238000004140 cleaning Methods 0.000 claims description 2
- 238000011010 flushing procedure Methods 0.000 claims description 2
- 239000011159 matrix material Substances 0.000 abstract description 8
- 239000013543 active substance Substances 0.000 abstract 1
- 239000007772 electrode material Substances 0.000 description 8
- 229910052799 carbon Inorganic materials 0.000 description 6
- 239000008367 deionised water Substances 0.000 description 6
- 229910021641 deionized water Inorganic materials 0.000 description 6
- 230000000694 effects Effects 0.000 description 6
- 238000007747 plating Methods 0.000 description 6
- 239000003054 catalyst Substances 0.000 description 4
- 238000005530 etching Methods 0.000 description 3
- 239000012535 impurity Substances 0.000 description 3
- 239000000463 material Substances 0.000 description 3
- 229910000510 noble metal Inorganic materials 0.000 description 3
- 238000010008 shearing Methods 0.000 description 3
- 238000005406 washing Methods 0.000 description 3
- 238000005265 energy consumption Methods 0.000 description 2
- 238000009776 industrial production Methods 0.000 description 2
- WOCIAKWEIIZHES-UHFFFAOYSA-N ruthenium(iv) oxide Chemical compound O=[Ru]=O WOCIAKWEIIZHES-UHFFFAOYSA-N 0.000 description 2
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 239000010411 electrocatalyst Substances 0.000 description 1
- 238000000840 electrochemical analysis Methods 0.000 description 1
- 239000006181 electrochemical material Substances 0.000 description 1
- 239000002803 fossil fuel Substances 0.000 description 1
- 238000010438 heat treatment Methods 0.000 description 1
- XLYOFNOQVPJJNP-ZSJDYOACSA-N heavy water Substances [2H]O[2H] XLYOFNOQVPJJNP-ZSJDYOACSA-N 0.000 description 1
- 150000002431 hydrogen Chemical class 0.000 description 1
- 229910052741 iridium Inorganic materials 0.000 description 1
- HTXDPTMKBJXEOW-UHFFFAOYSA-N iridium(IV) oxide Inorganic materials O=[Ir]=O HTXDPTMKBJXEOW-UHFFFAOYSA-N 0.000 description 1
- 238000011031 large-scale manufacturing process Methods 0.000 description 1
- 229910044991 metal oxide Inorganic materials 0.000 description 1
- 150000004706 metal oxides Chemical class 0.000 description 1
- 238000007254 oxidation reaction Methods 0.000 description 1
- 229910052760 oxygen Inorganic materials 0.000 description 1
- 239000001301 oxygen Substances 0.000 description 1
- 238000006722 reduction reaction Methods 0.000 description 1
- 229910052707 ruthenium Inorganic materials 0.000 description 1
- 238000001878 scanning electron micrograph Methods 0.000 description 1
- 150000003346 selenoethers Chemical class 0.000 description 1
- 150000003568 thioethers Chemical class 0.000 description 1
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- Electroplating Methods And Accessories (AREA)
Abstract
The invention discloses an electrolytic water hydrogen production electrode and a preparation method thereof, wherein a commercial electrode is subjected to electroetching in 1M HCl to obtain an electrode matrix with a rough surface, then the electrode matrix is used as a negative electrode to be electroplated, and a layer of NiCoP alloy active substance is covered on the surface of the electrode matrix.
Description
Technical Field
The invention relates to the technical field of electrochemical materials, in particular to a preparation method of an electrode for hydrogen production by water electrolysis.
Background
Increasing global energy demand and climate change due to over-utilization of fossil fuels have prompted a tightening search for various renewable energy sources. In particular, the electrolysis of water to produce hydrogen is considered to be one of the simplest and cleanest methods for producing hydrogen, but a higher overpotential is still required to obtain a better reaction rate. Industrial production has found that hydrogen production using an industrial electrolytic cell requires a potential of about 2V to drive with at least a 35% energy loss. At the same time the catalysts commonly used are still based on noble metals such as Pt-based alloys for hydrogen evolution and IrO2, RuO2 for oxygen evolution. The hydrogen production by electrolyzing water is difficult to realize large-scale production due to scarcity and high cost. Therefore, the preparation of highly active electrode materials to reduce the required potential is a problem to be solved.
At present, both noble metal (Ir and Ru) catalysts and non-noble metal catalysts including metal oxides, sulfides, selenides and phosphides have improved activity but the stability of the catalysts can not meet the requirements of industrial production. Ni-based electrocatalysts are commonly used as electrode materials for electrolysis of water because of their superior hydrogen evolution activity.
Disclosure of Invention
One of the purposes of the invention is to find a method for improving the activity of a Ni-based hydrogen evolution electrode of commercial electrolyzed water; the second objective is to find a lower cost material that can replace Ni-based electrodes. Firstly, an alloy material NiCoP similar to a spherical nanometer flower shape is grown on the surface of an electrode matrix by using a direct current electroplating method, so that the specific surface area and high-density active sites of the electrode matrix are improved, and then the alloy material NiCoP is further applied to an iron electrode and a copper electrode, so that the problems of high energy consumption, low activity and the like in the process of producing hydrogen by electrolyzing water through a commercial nickel net are solved, and the cost of the electrode material is greatly reduced.
In order to achieve the purpose, the invention relates to an electrode for producing hydrogen by electrolyzing water, which comprises an electrode substrate and NiCoP alloy covered on the surface of the electrode substrate.
The electrode substrate is an existing commercial metal electrode, preferably a nickel electrode, more preferably a copper electrode and an iron electrode, such as a copper mesh, a nickel mesh, a wire mesh.
The preparation method of the water electrolysis hydrogen production electrode specifically comprises the following steps:
(1) immersing the electrode substrate in HCl solution for electroetching until the reaction is complete, and then ultrasonically cleaning to remove HCl on the surface to obtain the electrode substrate with a rough surface;
(2) electroplating by using a two-electrode system, putting the electrode substrate treated in the step (1) into electroplating solution, applying constant current to electroplate the electrode substrate serving as a negative electrode and the graphite plate serving as a positive electrode, and flushing residual electroplating solution on the surface to obtain an electrode with the surface covered with alloy NiCoP, wherein the electroplating solution contains 0.1M NiCl2、0.1M CoCl2、0.1M NaH2PO2And 0.35M Na3C6H5O7。
In the electroplating process: the electrode matrix is used as a negative electrode to perform reduction reaction: ni2++2e-＝＝＝Ni，Co2++2e-＝＝＝Co，P3++3e-＝＝＝P，2H++2e-＝＝＝H2Forming NiCoP alloy on the surface of the electrode substrate, and taking the graphite plate as a positive electrode to perform oxidation reaction: 4OH--4e-＝＝＝O2+2H2O。
Specifically, in the step (1), an electrode matrix is immersed in 1M HCl solution, the electrode matrix is used as a positive electrode, a graphite plate is used as a negative electrode, and 50mAcm is applied-2The current density of (2) is electro-etched for 1 min.
Preferably, step (2) is at 500mAcm-2Electroplating for 1-3 min under the current density to ensure that the electrode material with the best performance is obtained.
Compared with the prior art, the invention has the following beneficial effects: (1) a layer of NiCoP alloy is electroplated on the surface of the commercial nickel screen, so that the hydrogen evolution activity of the material is greatly improved, and the energy consumption in the hydrogen production process is reduced. (2) Experimental results show that the NiCoP alloy can not only improve the performance of a nickel electrode, but also improve the performance of other metal electrodes, such as a copper electrode and an iron electrode, so that the universality of the method is proved, and better effects can be achieved by adopting the copper electrode and the iron electrode with lower cost as substrates under certain electroplating conditions. .
Drawings
FIG. 1 is an SEM photograph of the electrode material after Nickel Mesh (NM) plating for 2min in example 1, wherein the left image is magnified 200 times and the right image is magnified 50000 times.
Fig. 2 is an SEM image of the electrode material after 2min of the iron wire mesh (FM) plating in example 2, the left image is magnified 200 times and the right image is magnified 50000 times.
FIG. 3 is an SEM photograph of the electrode material after Copper Mesh (CM) plating for 2min in example 3, wherein the left side is magnified 200 times and the right side is magnified 20000 times.
FIG. 4 is a graph of HER performance after NiCoP 1, 2, 3min plating of the nickel mesh in example 1.
FIG. 5 is a graph of HER performance after wire mesh plating with NiCoP 1, 2, 3min in example 2.
FIG. 6 is a graph of HER performance after NiCoP 1, 2, 3min of copper mesh plating in example 3.
FIG. 7 is a graph comparing HER performance of samples prepared by electroplating for 2min in examples 1-3 with commercial nickel mesh.
FIG. 8 shows a sample prepared by electroplating for 2min in examples 1 to 3 and a commercial nickel screen of 10mAcm-2Overpotential map of (c).
Detailed Description
The invention is further illustrated by the following specific examples.
Example 1:
the preparation method of the electrode for hydrogen production by water electrolysis comprises the following steps:
immersing a nickel screen (NM) in 1M HCl solution, connecting the positive electrode of a power supply with the nickel screen, connecting the negative electrode of the power supply with a graphite plate, and keeping the power supply at 50mA cm-2Electroetching for 1min at the current density of (1X 1.5 cm), and shearing the electroetched nickel mesh2) Immersing in deionized water for 10min to remove the attached impurities on the surface;
taking out and directly immersing the carbon plate in electroplating solution to carry out electroplating by adopting a two-electrode system, wherein the cathode of a direct current power supply is connected with a nickel net, and the anode is connected with a carbon plate. Applying constant current (500 mAcm)-2) Respectively continuously etching 1, 2,3 min. And taking out after the completion, and washing the electrode with deionized water to obtain an electrode NiCoP/NM-1, an electrode NiCoP/NM-2 and an electrode NiCoP/NM-3 respectively. The electroplating solution contains 0.1M NiCl2、0.1M CoCl2、0.1M NaH2PO2And 0.35M Na3C6H5O7。
Example 2:
the preparation method of the electrode for hydrogen production by water electrolysis comprises the following steps:
immersing wire netting (FM) in 1M HCl solution, connecting the positive electrode of a power supply with the wire netting, connecting the negative electrode of the power supply with a graphite plate, and keeping the power supply at 50mA cm-2Electroetching at current density of (1) for 1min, and shearing commercial wire mesh (1 × 1.5 cm)2) Immersing in deionized water and ultrasonic treating for 10min to remove the attached impurities on the surface. Taking out and directly immersing the carbon plate in electroplating solution to carry out electroplating by adopting a two-electrode system, wherein the negative electrode of a direct current power supply is connected with a wire netting, and the positive electrode of the direct current power supply is connected with a carbon plate. Applying constant current (500mAcm-2) and etching for 1, 2 and 3min respectively. And taking out after the completion, and washing the electrode with deionized water to obtain an electrode NiCoP/FM-1, an electrode NiCoP/FM-2 and an electrode NiCoP/FM-3 respectively. The electroplating solution contains 0.1M NiCl2、0.1M CoCl2、0.1M NaH2PO2And 0.35M Na3C6H5O7。
Example 3:
the preparation method of the electrode for hydrogen production by water electrolysis comprises the following steps:
immersing copper mesh (NM) in 1M HCl solution, connecting positive electrode of power supply with copper mesh, connecting negative electrode with graphite plate, and heating at 50mA cm-2Electroetching for 1min at the current density of (1X 1.5 cm), and shearing off commercial copper mesh2) Immersing in deionized water and ultrasonic treating for 10min to remove the attached impurities on the surface. Taking out and directly immersing the carbon plate in electroplating solution to carry out electroplating by adopting a two-electrode system, wherein the negative electrode of a direct current power supply is connected with a copper net, and the positive electrode of the direct current power supply is connected with a carbon plate. Applying constant current (500 mAcm)-2) Etching is continued for 1, 2 and 3min respectively. And taking out after the completion, and washing the electrode with deionized water to obtain an electrode NiCoP/FM-1, an electrode NiCoP/FM-2 and an electrode NiCoP/FM-3 respectively. The electroplating solution contains 0.1M NiCl2、0.1M CoCl2、0.1M Na2H2PO2And 0.35M Na3C6H5O7。
Electrochemical tests were performed on the electrodes prepared in examples 1 to 3, respectively, and the results showed that: the electrode materials obtained in the embodiments 1-3 in the electroplating process for 2min have the best performance, and the universality of the NiCoP alloy material is proved, and the materials have excellent electrochemical hydrogen evolution performance.
As can be understood from fig. 7 and 8, under certain experimental conditions, the copper mesh and the iron mesh with the NiCoP alloy plated on the surface have better performance than the nickel mesh.
Claims (8)
1. The electrode for producing hydrogen by electrolyzing water is characterized by comprising an electrode substrate and NiCoP alloy covering the surface of the electrode substrate.
2. The water electrolysis hydrogen production electrode according to claim 1, wherein the electrode substrate is an existing commercial metal electrode substrate.
3. The electrode for producing hydrogen by electrolyzing water as claimed in claim 1, wherein the electrode substrate is a nickel electrode.
4. The electrode for producing hydrogen by electrolyzing water as claimed in claim 1, wherein the electrode substrate is a copper electrode or an iron electrode.
5. The preparation method of the electrode for hydrogen production by water electrolysis is characterized by comprising the following steps:
(1) immersing the electrode substrate in HCl solution for electroetching until the reaction is complete, and then ultrasonically cleaning to remove HCl on the surface to obtain the electrode substrate with a rough surface;
(2) electroplating by using a two-electrode system, placing the electrode substrate treated in the step (1) in electroplating solution, taking the electrode substrate as a negative electrode for electroplating, and flushing residual electroplating solution on the surface to obtain an electrode with the surface covered with alloy NiCoP, wherein the electroplating solution contains 0.1M NiCl2、0.1M CoCl2、0.1M NaH2PO2And 0.35M Na3C6H5O7。
6. The method for preparing the electrode for hydrogen production by electrolyzing water as claimed in claim 5, wherein the step (1) is to immerse the electrode substrate in 1M HCl solution, the electrode substrate is used as the positive electrode, the graphite plate is used as the negative electrode, and 50mA cm is applied-2The current density of (2) is electro-etched for 1 min.
7. The method for preparing the electrode for hydrogen production by electrolyzing water as claimed in claim 5, wherein the step (2) is performed at 500mAcm-2Electroplating for 1-3 min at the current density of (2).
8. The method for preparing the electrode for hydrogen production by electrolyzing water as claimed in claim 5, wherein the step (2) is performed at 500mAcm-2Electroplating for 2min at the current density of (2).
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Cited By (1)
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| CN115094460A (en) * | 2022-07-19 | 2022-09-23 | 同济大学 | Nickel-based composite electrode for alkaline electrolytic cell and preparation method thereof |
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