GB2623379A - Rapid preparation method of iron-doped nickel selenide, and use of iron-doped nickel selenide in cathode for water electrolysis - Google Patents

Rapid preparation method of iron-doped nickel selenide, and use of iron-doped nickel selenide in cathode for water electrolysis Download PDF

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Publication number
GB2623379A
GB2623379A GB2217503.8A GB202217503A GB2623379A GB 2623379 A GB2623379 A GB 2623379A GB 202217503 A GB202217503 A GB 202217503A GB 2623379 A GB2623379 A GB 2623379A
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United Kingdom
Prior art keywords
water electrolysis
iron
cathode
doped nickel
nickel selenide
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GB2217503.8A
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GB202217503D0 (en
Inventor
Chen Weiwu
Qin Zhaojun
Wang Zhiming
Zhao Runbo
Yao Yisen
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Yangtze River Delta Research Institute of UESTC Huzhou
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Yangtze River Delta Research Institute of UESTC Huzhou
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    • CCHEMISTRY; METALLURGY
    • C25ELECTROLYTIC OR ELECTROPHORETIC PROCESSES; APPARATUS THEREFOR
    • C25BELECTROLYTIC OR ELECTROPHORETIC PROCESSES FOR THE PRODUCTION OF COMPOUNDS OR NON-METALS; APPARATUS THEREFOR
    • C25B1/00Electrolytic production of inorganic compounds or non-metals
    • C25B1/01Products
    • C25B1/02Hydrogen or oxygen
    • C25B1/04Hydrogen or oxygen by electrolysis of water
    • BPERFORMING OPERATIONS; TRANSPORTING
    • B01PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01JCHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
    • B01J27/00Catalysts comprising the elements or compounds of halogens, sulfur, selenium, tellurium, phosphorus or nitrogen; Catalysts comprising carbon compounds
    • B01J27/02Sulfur, selenium or tellurium; Compounds thereof
    • B01J27/057Selenium or tellurium; Compounds thereof
    • B01J27/0573Selenium; Compounds thereof
    • CCHEMISTRY; METALLURGY
    • C25ELECTROLYTIC OR ELECTROPHORETIC PROCESSES; APPARATUS THEREFOR
    • C25BELECTROLYTIC OR ELECTROPHORETIC PROCESSES FOR THE PRODUCTION OF COMPOUNDS OR NON-METALS; APPARATUS THEREFOR
    • C25B11/00Electrodes; Manufacture thereof not otherwise provided for
    • C25B11/04Electrodes; Manufacture thereof not otherwise provided for characterised by the material
    • YGENERAL 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
    • Y02TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
    • Y02EREDUCTION OF GREENHOUSE GAS [GHG] EMISSIONS, RELATED TO ENERGY GENERATION, TRANSMISSION OR DISTRIBUTION
    • Y02E60/00Enabling technologies; Technologies with a potential or indirect contribution to GHG emissions mitigation
    • Y02E60/30Hydrogen technology
    • Y02E60/36Hydrogen production from non-carbon containing sources, e.g. by water electrolysis

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  • Chemical & Material Sciences (AREA)
  • Engineering & Computer Science (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • Materials Engineering (AREA)
  • Organic Chemistry (AREA)
  • Electrochemistry (AREA)
  • Metallurgy (AREA)
  • Inorganic Chemistry (AREA)
  • Electrolytic Production Of Non-Metals, Compounds, Apparatuses Therefor (AREA)

Abstract

A rapid preparation method of iron-doped nickel selenide, and use of the iron-doped nickel selenide in a cathode for water electrolysis is detailed. The preparation method includes the following steps: (1) preparing a ferric acetate-containing premixed solution; (2) immersing a nickel mesh into the premixed solution for a period of time, taking out, and drying by heating to obtain a ferric acetate-attached nickel mesh; (3) placing the ferric acetate-attached nickel mesh in a heating zone of a tubular furnace, and placing a selenium powder on an edge of the heating zone of the tubular furnace; and (4) conducting selenization to obtain the iron-doped nickel selenide that is directly connected to a water electrolysis device as a cathode for water electrolysis. The cathode for water electrolysis can be directly applied to a water electrolysis device. Ferric nitrate may be used in replacement for ferric acetate in conjunction with water rather than N,N-dimethylformamide in the premixed solution of step 1.

Description

RAPID PREPARATION METHOD OF IRON-DOPED NICKEL SELENIDE, AND USE OF IRON-DOPED NICKEL SELENIDE IN CATHODE FOR WATER ELECTROLYSIS
TECHNICAL FIELD
[0001] The present disclosure relates to the technical field of hydrogen production by water electrolysis, in particular to a preparation method of a photosensitive iron-doped nickel selenide cathode for water electrolysis.
BACKGROUND
[0002] Hydrogen has an extremely high specific energy, and has a combustion product of water only, which is an ideal fuel capable of replacing fossil energy. More importantly, hydrogen can be produced through water electrolysis, forming a clean closed loop from the decomposition of water to produce hydrogen to the combustion of hydrogen into water. However, the current hydrogen production by water electrolysis has a high cost and is difficult to conduct large-scale commercial production. Therefore, it is necessary to develop the hydrogen production by water electrolysis to efficiently produce high-purity hydrogen to meet market demands and replace fossil fuels such as coal.
[0003] The cost of hydrogen production by water electrolysis includes two parts: the first one is power consumption required in the hydrogen production by water electrolysis; and the second one is a cost of hydrogen production by water electrolysis device, including the cost of a cathode for water electrolysis, the cost of an anode for water electrolysis, and the cost of an electrolyte. Iron-doped nickel selenide is a material with desirable electrocatalytic activity and also a semiconductor material. It is known that semiconductor materials have a photoelectric effect under suitable light illumination, thereby increasing a carrier concentration on the surface of semiconductor materials. Therefore, the cathode for water electrolysis based on iron-doped nickel selenide is excited by light illumination, and photo-generated carriers obtained by the photoelectric effect improve electrical properties on a surface of the cathode for water electrolysis, thereby reducing the external power supply required for water electrolysis. On the other hand, a rapidly-prepared nickel selenide cathode for water electrolysis can effectively reduce a production cost of the cathode for water electrolysis, thus further reducing the cost of the hydrogen production by water electrolysis device.
SUMMARY
[0004] Aiming at the prior art, the present disclosure provides a rapid preparation method of a photosensitive iron-doped nickel selenide cathode for water electrolysis, so as to reduce a cost of a water electrolysis device and a power consumption during hydrogen production by water electrolysis.
[0005] To achieve the above objective, the technical solution adopted by the present disclosure is as follows: a rapid preparation method of a photosensitive iron-doped nickel selenide cathode for water electrolysis is provided, including the following steps: [0006] step 1: dissolving ferric acetate at a concentration of 0.2 g/mL into N,N-dimethylfonnamide to obtain a ferric acetate-containing premixed solution; [0007] step 2: immersing a nickel mesh into the premixed solution obtained in step 1 for 1 sec to 2 sec, taking out with tweezers, and drying in an oven or a heating platform at 60°C for 5 min to 10 min to obtain a ferric acetate-attached nickel mesh; [0008] step 3: placing the ferric acetate-attached nickel mesh obtained in step 2 in a heating zone of a tubular furnace, and placing a selenium powder on an edge of the heating zone of the tubular furnace; and [0009] step 4: conducting selenization in the heating zone of the tubular furnace at 480°C to 495°C for 5 min to 6 min to obtain the iron-doped nickel selenide that is directly connected to a water electrolysis device as a cathode for water electrolysis.
[0010] Preferably, the nickel mesh is immersed in the premixed solution for 1 sec and then taken out.
[0011] Preferably, the ferric acetate-attached nickel mesh is placed on the heating zone of the tubular furnace, and the selenium powder is placed on the edge of the heating zone of the tubular furnace; and selenization is conducted in the heating zone of the tubular furnace at 495°C for 5 min to obtain the iron-doped nickel selenide that is directly connected to the water electrolysis device without packaging as the cathode for water electrolysis.
[0012] Preferably, in step 1, ferric nitrate serves as an alternative to the ferric acetate, and water serves as an alternative to the N,N-dimethylformamide.
[0013] Preferably, the present disclosure further provides a photosensitive iron-doped nickel selenide cathode for water electrolysis prepared by the rapid preparation method of iron-doped nickel selenide. The cathode for water electrolysis is used as a cathode of a water electrolysis device for hydrogen production, showing obvious performance advantages; through the effect of solar energy, the cathode for water electrolysis has improved water electrolysis efficiency compared with the traditional cathodes for electrolysis water.
[0014] Preferably, the iron-doped nickel selenide cathode for water electrolysis is applied to an water electrolysis device; the water electrolysis device includes a cathode for water electrolysis, a graphite paper-based counter electrode, a reference electrode, and an electrolyte; the reference electrode is a Hg/Hg0 reference electrode; and the electrolyte is a potassium hydroxide solution with a pH value of 14. Through the photosensitive and iron-doped nickel selenide cathode for water electrolysis, a hydrogen production performance by water electrolysis of the water electrolysis device under light illumination is improved, thereby reducing the operating cost of the water electrolysis device.
[0015] The present disclosure has the beneficial effects as follows: in the present disclosure, the preparation method has simple conditions and a relatively short production time; by the preparation method of an iron-doped nickel selenide cathode for water electrolysis, a photosensitive iron-doped nickel selenide cathode for water electrolysis is obtained; the cathode for water electrolysis has a stable structure, a desirable catalytic activity, and a light sensitivity. When the iron-doped nickel selenide is used as the cathode for water electrolysis to produce hydrogen by water electrolysis, the iron-doped nickel selenide cathode for water electrolysis can be irradiated with sunlight to improve a hydrogen production efficiency, thereby reducing the electricity required for hydrogen production by water electrolysis.
BRIEF DESCRIPTION OF THE DRAWINGS
[0016] FIG. I shows a scanning electron microscopy (SEM) image of a photosensitive iron-doped nickel selenide cathode for water electrolysis; [0017] FIG. 2 shows an X-ray photoelectron energy spectrum of Fe on a surface of the photosensitive iron-doped nickel selenide cathode for water electrolysis; and 100181 FIG. 3 shows a polarization curve of the photosensitive iron-doped nickel selenide cathode for water electrolysis.
DETAILED DESCRIPTION OF THE EMBODIMENTS
[0019] The technical solutions of the embodiments of the present disclosure are clearly and completely described below with reference to the accompanying drawings. Apparently, the described embodiments are merely a part rather than all of the embodiments of the present disclosure. All other embodiments obtained by those of ordinary skill in the art based on the embodiments of the present disclosure without creative efforts shall fail within the protection scope of the present disclosure.
[0020] The present disclosure proposes a rapid preparation method of a photosensitive iron-doped nickel selenide cathode for water electrolysis, including the following steps: [0021] step 1: dissolving ferric acetate at a concentration of 0.2 g/mL into N,N-dimethylfonnamide to obtain a ferric acetate-containing premixed solution; [0022] step 2: immersing a nickel mesh into the premixed solution obtained in step 1 for 1 sec to 2 sec, taking out with tweezers, and drying in an oven or a heating platform at 60°C for S min to 10 min to obtain a ferric acetate-attached nickel mesh; 100231 step 3: placing the ferric acetate-attached nickel mesh obtained in step 2 in a heating zone of a tubular furnace, and placing a selenium powder on an edge of the heating zone of the tubular furnace; and 100241 step 4: conducting selenization in the heating zone of the tubular furnace at 480°C to 495°C for 5 min to 6 min to obtain the iron-doped nickel selenide that is directly connected to a water electrolysis device as a cathode for water electrolysis. The SEM image of FIG, t shows that the iron-doped nickel selenide cathode for water electrolysis obtained by the rapid preparation method has a stable wave structure, and the void structure of the nickel mesh still exists. This provides a huge specific surface area and a large number of active sites for the iron-doped nickel selenide cathode for water electrolysis.
100251 Further, the nickel mesh is immersed in the premixed solution for 1 sec and then taken out.
100261 Further, the ferric acetate-attached nickel mesh is placed on the heating zone of the tubular furnace, and the selenium powder is placed on the edge of the heating zone of the tubular furnace; and selenization is conducted in the heating zone of the tubular furnace at 495°C for 5 min to obtain the iron-doped nickel selenide that is directly connected to the water electrolysis device without packaging as the cathode for water electrolysis. The X-ray photoelectron spectrum of the Fe element in FIG. 2 shows that the Fe element has been successfully doped into the nickel selenide lattice. Compared with the standard X-ray photoelectron spectrum of Fe element, it can be determined that the Fe element in the iron-doped nickel selenide cathode for water electrolysis is in a positive trivalent state.
100271 Further, in step I, ferric nitrate may serve as an alternative to the ferric acetate, and water may serve as an alternative to the N,N-dimethylformamide.
100281 Further, the present disclosure further provides a photosensitive iron-doped nickel selenide cathode for water electrolysis prepared by the preparation method of a photosensitive iron-doped nickel selenide cathode for water electrolysis.
100291 Further, the present disclosure further provides use of the photosensitive iron-doped nickel selenide cathode for water electrolysis, where the iron-doped nickel selenide cathode for water electrolysis is applied to an water electrolysis device; the water electrolysis device includes a cathode for water electrolysis, a graphite paper-based counter electrode, a reference electrode, and an electrolyte; the reference electrode is a Hg/Hg0 reference electrode; and the electrolyte is a potassium hydroxide solution with a pH value of 14. The polarization curve in FIG. 3 shows that when the photosensitive iron-doped nickel selenide cathode for water electrolysis is applied with an overpotentia1 of 150 mV, a current density generated on the electrode is 32.6 mA/cm2.
After applying light illumination to the photosensitive iron-doped nickel selenide cathode for water electrolysis, the current density is increased to 42.1 mA/cm2 under the same overpotential of 150 mV, with an increase of 29.1%.
100301 The embodiments of the present disclosure will be described below in detail in conjunction with examples, but should not be construed as limiting the scope of the disclosure. Within the scope of the claims, all modifications and variations made by those skilled in the art without creative efforts shall fall within the protection scope of the present disclosure.

Claims (6)

  1. WHAT IS CLAIMED IS: I. A rapid preparation method of iron-doped nickel selenide, comprising the following steps: step 1: dissolving ferric acetate at a concentration of 0.2 g/mL into N,N-dimethylformamide to obtain a ferric acetate-containing premixed solution; step 2: immersing a nickel mesh into the premixed solution obtained in step 1 for 1 sec to 2 sec, taking out with tweezers, and drying in an oven or a heating platform at 60°C for 5 min to 10 min to obtain a ferric acetate-attached nickel mesh; step 3: placing the ferric acetate-attached nickel mesh obtained in step 2 in a heating zone of a tubular furnace, and placing a selenium powder on an edge of the heating zone of the tubular furnace; and step 4: conducting selenization in the heating zone of the tubular furnace at 480°C to 495°C for 5 min to 6 min to obtain the iron-doped nickel selenide that is directly connected to a water electrolysis device as a cathode for water electrolysis.
  2. 2. The rapid preparation method of iron-doped nickel selenide according to claim I, wherein the nickel mesh is immersed in the premixed solution for 1 sec and then taken out.
  3. 3. The rapid preparation method of iron-doped nickel selenide according to claim I, wherein the ferric acetate-attached nickel mesh is placed on the heating zone of the tubular furnace, and the selenium powder is placed on the edge of the heating zone of the tubular furnace; and selenization is conducted in the heating zone of the tubular furnace at 495°C for 5 min to obtain the iron-doped nickel selenide that is directly connected to the water electrolysis device without packaging as the cathode for water electrolysis.
  4. 4. The rapid preparation method of iron-doped nickel selenide according to claim 1, wherein in step 1, ferric nitrate serves as an alternative to the ferric acetate, and water serves as an alternative to the N,N-dimethylformamide
  5. 5. A photosensitive iron-doped nickel selenide cathode for water electrolysis prepared by the rapid preparation method of iron-doped nickel selenide according to any one of claims 1 to 4.
  6. 6. Use of the iron-doped nickel selenide according to claim 5 in a cathode for water electrolysis, wherein the iron-doped nickel selenide cathode for water electrolysis is applied in a water electrolysis device; the water electrolysis device comprises a cathode for water electrolysis, a graphite paper-based counter electrode, a reference electrode, and an electrolyte; the reference electrode is a Hg/Hg0 reference electrode, and the electrolyte is a potassium hydroxide solution with a pH value of 14.S
GB2217503.8A 2022-10-12 2022-11-23 Rapid preparation method of iron-doped nickel selenide, and use of iron-doped nickel selenide in cathode for water electrolysis Pending GB2623379A (en)

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Citations (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN109954503A (en) * 2019-03-28 2019-07-02 浙江大学 A kind of nickelous selenide and ternary selenizing ferronickel composite electrocatalyst and preparation method and application
CN115172677A (en) * 2022-05-13 2022-10-11 南京大学 Preparation method of iron-doped nickel selenide nano material, obtained product and application

Patent Citations (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN109954503A (en) * 2019-03-28 2019-07-02 浙江大学 A kind of nickelous selenide and ternary selenizing ferronickel composite electrocatalyst and preparation method and application
CN115172677A (en) * 2022-05-13 2022-10-11 南京大学 Preparation method of iron-doped nickel selenide nano material, obtained product and application

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