CN112795952A - Porous NiCu nanoneedle array catalyst and preparation method thereof - Google Patents
Porous NiCu nanoneedle array catalyst and preparation method thereof Download PDFInfo
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- CN112795952A CN112795952A CN202110134183.6A CN202110134183A CN112795952A CN 112795952 A CN112795952 A CN 112795952A CN 202110134183 A CN202110134183 A CN 202110134183A CN 112795952 A CN112795952 A CN 112795952A
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- 229910003322 NiCu Inorganic materials 0.000 title claims abstract description 63
- 239000003054 catalyst Substances 0.000 title claims abstract description 35
- 238000002360 preparation method Methods 0.000 title claims abstract description 20
- 239000000463 material Substances 0.000 claims abstract description 16
- 238000000034 method Methods 0.000 claims abstract description 10
- 239000000956 alloy Substances 0.000 claims description 17
- 229910045601 alloy Inorganic materials 0.000 claims description 17
- 229910021607 Silver chloride Inorganic materials 0.000 claims description 15
- 238000005530 etching Methods 0.000 claims description 15
- HKZLPVFGJNLROG-UHFFFAOYSA-M silver monochloride Chemical compound [Cl-].[Ag+] HKZLPVFGJNLROG-UHFFFAOYSA-M 0.000 claims description 15
- 229910021642 ultra pure water Inorganic materials 0.000 claims description 10
- 239000012498 ultrapure water Substances 0.000 claims description 10
- 230000004913 activation Effects 0.000 claims description 9
- CSCPPACGZOOCGX-UHFFFAOYSA-N Acetone Chemical compound CC(C)=O CSCPPACGZOOCGX-UHFFFAOYSA-N 0.000 claims description 8
- 238000004140 cleaning Methods 0.000 claims description 8
- 238000001035 drying Methods 0.000 claims description 7
- PCHJSUWPFVWCPO-UHFFFAOYSA-N gold Chemical compound [Au] PCHJSUWPFVWCPO-UHFFFAOYSA-N 0.000 claims description 6
- 239000010931 gold Substances 0.000 claims description 6
- 229910052737 gold Inorganic materials 0.000 claims description 6
- 229910052802 copper Inorganic materials 0.000 claims description 5
- 229910052759 nickel Inorganic materials 0.000 claims description 5
- 238000002844 melting Methods 0.000 claims description 3
- 230000008018 melting Effects 0.000 claims description 3
- 238000010891 electric arc Methods 0.000 claims description 2
- 239000003792 electrolyte Substances 0.000 claims 2
- 230000003213 activating effect Effects 0.000 claims 1
- 238000005406 washing Methods 0.000 claims 1
- 239000001257 hydrogen Substances 0.000 abstract description 15
- 229910052739 hydrogen Inorganic materials 0.000 abstract description 15
- UFHFLCQGNIYNRP-UHFFFAOYSA-N Hydrogen Chemical compound [H][H] UFHFLCQGNIYNRP-UHFFFAOYSA-N 0.000 abstract description 14
- 230000003197 catalytic effect Effects 0.000 abstract description 14
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 abstract description 11
- 238000006243 chemical reaction Methods 0.000 abstract description 9
- 229910018054 Ni-Cu Inorganic materials 0.000 abstract description 8
- 229910018481 Ni—Cu Inorganic materials 0.000 abstract description 8
- 239000007772 electrode material Substances 0.000 abstract description 7
- 238000005868 electrolysis reaction Methods 0.000 abstract description 6
- 238000005516 engineering process Methods 0.000 abstract description 6
- 238000004519 manufacturing process Methods 0.000 abstract description 6
- 230000000694 effects Effects 0.000 abstract description 4
- 229910000510 noble metal Inorganic materials 0.000 abstract description 4
- 238000011160 research Methods 0.000 abstract description 4
- 238000002048 anodisation reaction Methods 0.000 abstract description 3
- 238000000354 decomposition reaction Methods 0.000 abstract description 2
- 238000004134 energy conservation Methods 0.000 abstract 1
- 229910052751 metal Inorganic materials 0.000 description 3
- 238000011161 development Methods 0.000 description 2
- XLYOFNOQVPJJNP-UHFFFAOYSA-M hydroxide Chemical compound [OH-] XLYOFNOQVPJJNP-UHFFFAOYSA-M 0.000 description 2
- 239000002184 metal Substances 0.000 description 2
- 238000010791 quenching Methods 0.000 description 2
- 230000000171 quenching effect Effects 0.000 description 2
- 238000001179 sorption measurement Methods 0.000 description 2
- 238000009718 spray deposition Methods 0.000 description 2
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 description 1
- 239000011865 Pt-based catalyst Substances 0.000 description 1
- 238000002441 X-ray diffraction Methods 0.000 description 1
- 238000005275 alloying Methods 0.000 description 1
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 description 1
- 230000006399 behavior Effects 0.000 description 1
- 238000006555 catalytic reaction Methods 0.000 description 1
- 238000002485 combustion reaction Methods 0.000 description 1
- 150000001875 compounds Chemical class 0.000 description 1
- 230000002596 correlated effect Effects 0.000 description 1
- 238000002484 cyclic voltammetry Methods 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- 230000006866 deterioration Effects 0.000 description 1
- 238000010494 dissociation reaction Methods 0.000 description 1
- 230000005593 dissociations Effects 0.000 description 1
- 238000000724 energy-dispersive X-ray spectrum Methods 0.000 description 1
- 238000003912 environmental pollution Methods 0.000 description 1
- 150000002431 hydrogen Chemical class 0.000 description 1
- 125000002887 hydroxy group Chemical group [H]O* 0.000 description 1
- 238000009776 industrial production Methods 0.000 description 1
- 210000003041 ligament Anatomy 0.000 description 1
- 239000001301 oxygen Substances 0.000 description 1
- 229910052760 oxygen Inorganic materials 0.000 description 1
- 230000010287 polarization Effects 0.000 description 1
- 239000002243 precursor Substances 0.000 description 1
- 239000002994 raw material Substances 0.000 description 1
- 238000012827 research and development Methods 0.000 description 1
- 238000001878 scanning electron micrograph Methods 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
- 239000012085 test solution Substances 0.000 description 1
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Classifications
-
- C—CHEMISTRY; METALLURGY
- C25—ELECTROLYTIC OR ELECTROPHORETIC PROCESSES; APPARATUS THEREFOR
- C25B—ELECTROLYTIC OR ELECTROPHORETIC PROCESSES FOR THE PRODUCTION OF COMPOUNDS OR NON-METALS; APPARATUS THEREFOR
- C25B1/00—Electrolytic production of inorganic compounds or non-metals
- C25B1/01—Products
- C25B1/02—Hydrogen or oxygen
- C25B1/04—Hydrogen or oxygen by electrolysis of water
-
- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02E—REDUCTION OF GREENHOUSE GAS [GHG] EMISSIONS, RELATED TO ENERGY GENERATION, TRANSMISSION OR DISTRIBUTION
- Y02E60/00—Enabling technologies; Technologies with a potential or indirect contribution to GHG emissions mitigation
- Y02E60/30—Hydrogen technology
- Y02E60/36—Hydrogen production from non-carbon containing sources, e.g. by water electrolysis
Abstract
The invention relates to a preparation method of an electrochemical catalyst for hydrogen production by water decomposition, belonging to the technical field of energy conversion material preparation. In the water electrolysis hydrogen production technology, the electrode material with high activity can effectively reduce the reaction kinetics obstruction, thereby achieving the purpose of energy conservation. Among them, Ni-Cu based materials have good catalytic performance and are the hot points of research in recent years. However, the existing Ni-Cu based materials are limited by insufficient number of active sites, and the catalytic activity is different from that of the noble metal Pt catalyst. The invention aims to further increase the number of active sites of a Ni-Cu-based material, adopts an electrochemical etching-electrochemical anodization method, and provides a porous NiCu nanoneedle array catalyst and a preparation method thereof, wherein the catalyst has a current density of 10 mA-cm when a hydrogen evolution reaction is carried out in 0.1M KOH‑2The overpotential at this time was 92mV (vs. RHE).
Description
Technical Field
The invention relates to the technical field of catalyst material preparation, and provides a porous NiCu nanoneedle array catalyst applicable to hydrogen production by water electrolysis and a preparation method thereof.
Background
With the exhaustion of traditional fossil energy and the deterioration of natural environment, the development of sustainable clean energy becomes a research hotspot. Hydrogen has high energy density and good compressibility, and the only combustion product is water, which will not cause environmental pollution, and is one of the most promising new energy sources to replace the traditional fossil energy sources in the future. The water electrolysis hydrogen production technology can utilize water as a raw material to prepare hydrogen, and is widely concerned. The water electrolysis hydrogen production technology depends on an electrode material with excellent catalytic performance. The electrode material with the best performance is mainly Pt-based, so that the economic cost is too high and the industrial production is difficult. Therefore, the research and development of the non-noble metal catalytic electrode material with reasonable cost and high catalytic activity has important value.
The electrolytic water reaction consists of two half-reactions, the Hydrogen Evolution Reaction (HER) and the Oxygen Evolution Reaction (OER), and the development of catalytic electrode materials is usually carried out for one or both half-reactions. Among non-noble metals, Ni is widely studied because of its good hydrogen evolution activity. A large number of researches show that compared with a single-metal Ni material, the binary or multi-element catalyst prepared by alloying can have more excellent hydrogen evolution activity. Therefore, a preparation method using Ni as one of the main components and introducing other metal elements has been a focus of research. According to the Norskov adsorption energy theory and a Sabatier intermediate compound model, the combination of Cu element and Ni element can obtain the hydrogen evolution catalytic electrode material with excellent performance. There are currently a large number of reports of Ni-Cu based HER catalytic materials. Although the HER catalytic activity of Ni-Cu based materials is good, there is still a certain distance from the noble metal Pt-based catalysts. At present, the weak link of the Ni-Cu base material is insufficient in active sites, so that the catalytic capability of the Ni-Cu base material can be improved around the weak link.
Disclosure of Invention
The invention aims to overcome the defects of the existing Ni-Cu-based HER catalytic material and provides a porous NiCu nanoneedle array catalyst and a preparation technology thereof. The invention adopts the method of electrochemical etching-electrochemical anodization, firstly utilizes Ni and Cu at 0.5M H2SO4And (3) carrying out electrochemical etching on the NiCu master alloy strip according to the difference of the electrochemical behaviors, and selectively etching away a part of Cu to prepare the porous NiCu material. Because the surface of the catalyst is distributed with the NiCu metal ligaments which are mutually connected and the nano holes with different sizes, the catalytic performance is obviously improved. The porous NiCu was then exposed to 1M KOHAnd (4) carrying out polarization treatment to prepare the porous NiCu nanoneedle array catalyst. The oxide/hydroxide of Ni and Cu introduced by the anodization can effectively accelerate the dissociation of water and the adsorption of hydroxyl substances, and improve the hydrogen evolution activity of the catalyst in an alkaline environment. Meanwhile, the porous morphology is activated into a nano needle array, so that the active specific surface area is optimized, more active sites are exposed, and the water decomposition reaction is promoted. The catalyst prepared by the method can be used as an electrode material to efficiently catalyze the hydrogen production reaction by water electrolysis, and has potential application to other similar electrolysis and catalysis systems. The technical scheme of the invention is as follows:
(1) preparation of NiCu master alloy strip (NiCu)
The high-purity Cu and Ni ingot is made into NiCu master alloy according to the atomic ratio of 1:1 by utilizing an electric arc melting technology. The master alloy ingot was rapidly solidified using a single roll rotary quenching and spray casting system to produce a NiCu master alloy strip (1X 0.2 cm)2) And a thickness of about 30 μm.
(2) Preparation of porous NiCu (p-NiCu)
And ultrasonically cleaning the prepared NiCu master alloy strip by using acetone and ultrapure water in sequence, and connecting the dried NiCu master alloy strip with an electrochemical workstation to be used as a working electrode in a three-electrode system. The gold flakes were treated in the same way at the same time and used as auxiliary electrodes; Ag/AgCl electrode as reference electrode at 0.5M H2SO4Performing electrochemical etching. The etching voltage is 1.0V (vs. Ag/AgCl), and the etching time is 300 s. And after etching, cleaning the prepared porous NiCu for 3 times by using ultrapure water, and naturally drying at room temperature.
(3) Preparation of porous NiCu nanoneedle array catalyst (p-NiCu NAs)
And connecting the porous NiCu prepared in the last step with an electrochemical workstation to be used as a working electrode in a three-electrode system, using a cleaned gold sheet as an auxiliary electrode, using an Ag/AgCl electrode as a reference electrode, and carrying out anode activation on the porous NiCu in 1M KOH. The activation voltage was 0.6V (vs. Ag/AgCl) and the activation time was 400 s. And (3) cleaning the activated material, namely the porous NiCu nanoneedle array catalyst, with ultrapure water for 3 times, and naturally drying at room temperature.
Drawings
FIG. 1 is an SEM image of a NiCu master alloy (b) porous NiCu (c) and porous NiCu nanoneedle array catalyst;
FIG. 2 is a related XRD pattern;
FIG. 3(a) EDS spectra of porous NiCu nanoneedle array catalyst;
FIG. 4 is a graph of hydrogen evolution LSV of a porous NiCu nanoneedle array catalyst in 0.1M KOH;
FIG. 5 CV graphs (test solution 0.1M KOH) for each catalyst in the non-faradaic zone; (d) current density versus scan rate.
Detailed Description
The invention provides a porous NiCu nanoneedle array catalyst and a preparation method thereof, and the specific implementation mode is as follows.
And respectively ultrasonically cleaning the high-purity Cu and Ni ingots by acetone, absolute ethyl alcohol and ultrapure water for 20min, and preparing the NiCu master alloy by using an arc melting technology according to an atomic ratio of 1: 1. The master alloy ingot was rapidly solidified using a single roll rotary quenching and spray casting system to produce a NiCu master alloy strip (1X 0.2 cm)2) And a thickness of about 30 μm.
And respectively ultrasonically cleaning the prepared NiCu master alloy strip for 20min by using acetone and ultrapure water, drying, and connecting with an electrochemical workstation to be used as a working electrode in a three-electrode system. The gold flakes were treated in the same way at the same time and used as auxiliary electrodes; Ag/AgCl electrode as reference electrode at 0.5M H2SO4Performing electrochemical etching. The etching voltage is 1.0V (vs. Ag/AgCl), and the etching time is 300 s. And after etching, cleaning the prepared porous NiCu with ultrapure water for 3 times, each time for 20min, and naturally drying at room temperature.
And connecting the porous NiCu prepared in the last step with an electrochemical workstation to serve as a working electrode in a three-electrode system, wherein a gold sheet serves as an auxiliary electrode, and an Ag/AgCl electrode serves as a reference electrode. The porous NiCu was anodically activated in 1M KOH. The activation voltage was 0.6V (vs. Ag/AgCl) and the activation time was 400 s. The material after activation is porous NiCu nanometer needle array catalyst (p-NiCu NAs), washed with ultrapure water for 3 times, each time for 20min, and naturally dried at room temperature.
To test the catalytic activity of the material, LSV test was performed in 0.1M KOH (pH 13) using a porous NiCu nanoneedle array catalyst as the working electrode, gold plate as the auxiliary electrode, and Ag/AgCl electrode as the reference electrode. The test potential window is-0.9 to-1.4V (vs. Ag/AgCl), and the scanning speed is 2 mV.s-1And converting the current to a current density. The test results are shown in fig. 4 (experimental data IR compensated). The calculated Tafel slope of the porous NiCu nanoneedle array catalyst is 66mV dec-1The initial overpotential was 52mV and the current density was 10mA cm-2The overpotential was 92 mV.
To compare the electrochemical active areas of the porous NiCu nanoneedle array catalyst and its precursor, scanning was performed in 0.1M KOH using cyclic voltammetry in the non-Faraday interval (0.02, 0.04, 0.06, 0.08, 0.1 V.s)-1) And calculating the electric double layer capacitance (C) positively correlated to the electrochemically active areadl) The results obtained are shown in FIG. 5. As shown in the figure, the porous NiCu nanoneedle array catalyst exhibited the highest CdlValue of about 12mF cm-2Is 8 times that of the porous NiCu, and is more than 120 times that of the NiCu master alloy. The experimental phenomenon proves that the introduction of the oxide/hydroxide increases the active sites of the porous NiCu, and the obtained porous NiCu nanoneedle array catalyst has more excellent HER catalytic performance.
Claims (5)
1. A porous NiCu nanoneedle array catalyst and a preparation method thereof are characterized by comprising the following steps:
(1) preparation of NiCu master alloy strip
High-purity Ni and Cu are prepared into NiCu master alloy strips (1 multiplied by 0.2 cm) according to the atomic ratio of 1:1 by adopting an electric arc melting method2) A thickness of about 30 μm;
(2) preparation of porous NiCu
Ultrasonically cleaning the obtained NiCu mother alloy strip with acetone and ultrapure water for 20min, drying, connecting with an electrochemical workstation, using as a working electrode in a three-electrode system, treating gold sheet with the same method, using as an auxiliary electrode, using Ag/AgCl electrode as a reference electrode, and placing in a 0.5M H container2SO4Carrying out electrochemical etching, wherein the etching voltage is 1.0V (vs. Ag/AgCl), the etching time is 300s, after the etching is finished, cleaning the prepared porous NiCu with ultrapure water for 3 times, each time for 20min, and naturally drying at room temperature;
(3) preparation of porous NiCu nanoneedle array catalyst
And connecting the prepared porous NiCu with an electrochemical workstation to serve as a working electrode in a three-electrode system by adopting the same method as the previous step, putting the porous NiCu in 1M KOH for anode activation, wherein the activation voltage is 0.6V (vs. Ag/AgCl), the activation time is 400s, the activated material is the porous NiCu nanoneedle array catalyst, washing the porous NiCu nanoneedle array catalyst for 3 times by using ultrapure water, each time for 20min, and naturally drying the porous NiCu at room temperature.
2. The preparation method of the porous NiCu nanoneedle array catalyst according to claim 1, wherein the process parameters in the step (1) are as follows: cu to Ni atomic ratio 1:1, NiCu master alloy strip (1X 0.2 cm)2) And a thickness of about 30 μm.
3. The preparation method of the porous NiCu nanoneedle array catalyst according to claim 1, wherein the process parameters in the step (2) are as follows: etching electrolyte was 0.5M H2SO4The voltage was 1.0V (vs. Ag/AgCl) and the time was 300 s.
4. The preparation method of the porous NiCu nanoneedle array catalyst according to claim 1, wherein the process parameters in the step (3) are as follows: the activating electrolyte was 1M KOH, voltage 0.6V (vs. Ag/AgCl), time 400 s.
5. A porous NiCu nanoneedle array catalyst prepared according to the method of any one of claims 1 to 4.
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN114250486A (en) * | 2022-01-20 | 2022-03-29 | 西南石油大学 | Preparation method of surface nano-porous NiMoCu catalyst |
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| CN111108233A (en) * | 2017-09-21 | 2020-05-05 | 海默斯有限公司 | Method for producing electrocatalyst |
| CN111041303A (en) * | 2018-10-13 | 2020-04-21 | 天津大学 | Method for preparing Ti-Cu-Ni porous material by using amorphous alloy and application thereof |
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN114250486A (en) * | 2022-01-20 | 2022-03-29 | 西南石油大学 | Preparation method of surface nano-porous NiMoCu catalyst |
| CN114250486B (en) * | 2022-01-20 | 2024-02-20 | 西南石油大学 | Preparation method of surface nano porous NiMoCu catalyst |
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