CN115928117A - Preparation method of iron-doped coralline heterostructure catalyst - Google Patents
Preparation method of iron-doped coralline heterostructure catalyst Download PDFInfo
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- CN115928117A CN115928117A CN202210635460.6A CN202210635460A CN115928117A CN 115928117 A CN115928117 A CN 115928117A CN 202210635460 A CN202210635460 A CN 202210635460A CN 115928117 A CN115928117 A CN 115928117A
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- 239000003054 catalyst Substances 0.000 title claims abstract description 36
- 238000002360 preparation method Methods 0.000 title claims abstract description 9
- PXHVJJICTQNCMI-UHFFFAOYSA-N Nickel Chemical compound [Ni] PXHVJJICTQNCMI-UHFFFAOYSA-N 0.000 claims abstract description 62
- 229910052759 nickel Inorganic materials 0.000 claims abstract description 25
- YGHCWPXPAHSSNA-UHFFFAOYSA-N nickel subsulfide Chemical compound [Ni].[Ni]=S.[Ni]=S YGHCWPXPAHSSNA-UHFFFAOYSA-N 0.000 claims abstract description 18
- LYCAIKOWRPUZTN-UHFFFAOYSA-N Ethylene glycol Chemical compound OCCO LYCAIKOWRPUZTN-UHFFFAOYSA-N 0.000 claims description 59
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 34
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 24
- UMGDCJDMYOKAJW-UHFFFAOYSA-N thiourea Chemical compound NC(N)=S UMGDCJDMYOKAJW-UHFFFAOYSA-N 0.000 claims description 22
- FBXVOTBTGXARNA-UHFFFAOYSA-N bismuth;trinitrate;pentahydrate Chemical compound O.O.O.O.O.[Bi+3].[O-][N+]([O-])=O.[O-][N+]([O-])=O.[O-][N+]([O-])=O FBXVOTBTGXARNA-UHFFFAOYSA-N 0.000 claims description 12
- 238000001035 drying Methods 0.000 claims description 12
- XSQUKJJJFZCRTK-UHFFFAOYSA-N Urea Natural products NC(N)=O XSQUKJJJFZCRTK-UHFFFAOYSA-N 0.000 claims description 11
- NQXWGWZJXJUMQB-UHFFFAOYSA-K iron trichloride hexahydrate Chemical compound O.O.O.O.O.O.[Cl-].Cl[Fe+]Cl NQXWGWZJXJUMQB-UHFFFAOYSA-K 0.000 claims description 11
- WGCNASOHLSPBMP-UHFFFAOYSA-N hydroxyacetaldehyde Natural products OCC=O WGCNASOHLSPBMP-UHFFFAOYSA-N 0.000 claims description 10
- 238000005406 washing Methods 0.000 claims description 9
- 238000000034 method Methods 0.000 claims description 6
- 238000004140 cleaning Methods 0.000 claims description 3
- 239000006260 foam Substances 0.000 claims description 3
- 239000000203 mixture Substances 0.000 claims description 3
- 229940044631 ferric chloride hexahydrate Drugs 0.000 claims 1
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 abstract description 23
- 238000006243 chemical reaction Methods 0.000 abstract description 23
- 229910052760 oxygen Inorganic materials 0.000 abstract description 23
- 239000001301 oxygen Substances 0.000 abstract description 23
- 239000000463 material Substances 0.000 abstract description 22
- XEEYBQQBJWHFJM-UHFFFAOYSA-N Iron Chemical compound [Fe] XEEYBQQBJWHFJM-UHFFFAOYSA-N 0.000 abstract description 10
- 230000000694 effects Effects 0.000 abstract description 9
- 229910052742 iron Inorganic materials 0.000 abstract description 4
- 230000003197 catalytic effect Effects 0.000 abstract description 3
- 238000001027 hydrothermal synthesis Methods 0.000 abstract description 3
- 238000003795 desorption Methods 0.000 abstract description 2
- RGKSCFKZOUGILU-UHFFFAOYSA-N [Bi](=S)=S Chemical compound [Bi](=S)=S RGKSCFKZOUGILU-UHFFFAOYSA-N 0.000 abstract 1
- 238000010923 batch production Methods 0.000 abstract 1
- 238000009826 distribution Methods 0.000 abstract 1
- 230000002349 favourable effect Effects 0.000 abstract 1
- NKHCNALJONDGSY-UHFFFAOYSA-N nickel disulfide Chemical compound [Ni+2].[S-][S-] NKHCNALJONDGSY-UHFFFAOYSA-N 0.000 abstract 1
- 231100000956 nontoxicity Toxicity 0.000 abstract 1
- CSCPPACGZOOCGX-UHFFFAOYSA-N Acetone Chemical compound CC(C)=O CSCPPACGZOOCGX-UHFFFAOYSA-N 0.000 description 14
- VEXZGXHMUGYJMC-UHFFFAOYSA-N Hydrochloric acid Chemical compound Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 description 14
- 230000000052 comparative effect Effects 0.000 description 14
- UFHFLCQGNIYNRP-UHFFFAOYSA-N Hydrogen Chemical compound [H][H] UFHFLCQGNIYNRP-UHFFFAOYSA-N 0.000 description 8
- 229910052739 hydrogen Inorganic materials 0.000 description 8
- 239000001257 hydrogen Substances 0.000 description 8
- 238000003487 electrochemical reaction Methods 0.000 description 6
- 238000004506 ultrasonic cleaning Methods 0.000 description 6
- 238000002441 X-ray diffraction Methods 0.000 description 5
- 238000000354 decomposition reaction Methods 0.000 description 4
- 238000004519 manufacturing process Methods 0.000 description 4
- 238000001878 scanning electron micrograph Methods 0.000 description 4
- 235000014653 Carica parviflora Nutrition 0.000 description 3
- 241000243321 Cnidaria Species 0.000 description 3
- 238000003917 TEM image Methods 0.000 description 3
- 238000006555 catalytic reaction Methods 0.000 description 2
- 230000008859 change Effects 0.000 description 2
- 239000003792 electrolyte Substances 0.000 description 2
- 230000007613 environmental effect Effects 0.000 description 2
- 150000004706 metal oxides Chemical class 0.000 description 2
- 229910000510 noble metal Inorganic materials 0.000 description 2
- 230000010287 polarization Effects 0.000 description 2
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 description 1
- 229910001030 Iron–nickel alloy Inorganic materials 0.000 description 1
- 229910021607 Silver chloride Inorganic materials 0.000 description 1
- 230000009471 action Effects 0.000 description 1
- 230000004075 alteration Effects 0.000 description 1
- 230000004888 barrier function Effects 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 230000033228 biological regulation Effects 0.000 description 1
- 229910052799 carbon Inorganic materials 0.000 description 1
- 239000007809 chemical reaction catalyst Substances 0.000 description 1
- 238000002485 combustion reaction Methods 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- 239000008367 deionised water Substances 0.000 description 1
- 229910021641 deionized water Inorganic materials 0.000 description 1
- 239000010411 electrocatalyst Substances 0.000 description 1
- 239000002803 fossil fuel Substances 0.000 description 1
- 238000009776 industrial production Methods 0.000 description 1
- 239000002135 nanosheet Substances 0.000 description 1
- 229910052755 nonmetal Inorganic materials 0.000 description 1
- BASFCYQUMIYNBI-UHFFFAOYSA-N platinum Chemical compound [Pt] BASFCYQUMIYNBI-UHFFFAOYSA-N 0.000 description 1
- 230000008569 process Effects 0.000 description 1
- HKZLPVFGJNLROG-UHFFFAOYSA-M silver monochloride Chemical compound [Cl-].[Ag+] HKZLPVFGJNLROG-UHFFFAOYSA-M 0.000 description 1
- 239000002904 solvent Substances 0.000 description 1
- 238000003860 storage Methods 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
- 238000006467 substitution reaction Methods 0.000 description 1
- 230000007704 transition Effects 0.000 description 1
- 230000037303 wrinkles Effects 0.000 description 1
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- 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
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Abstract
The invention discloses a preparation method of an iron-doped coralliform heterostructure catalyst, which successfully realizes the controllable doping of iron in a Ni3S2/Bi3S2 heterostructure by one-step hydrothermal process, the material has a highly-folded microstructure, high conductivity and high specific surface area, provides more active sites, and the three-dimensional multilayer structure is favorable for the desorption of oxygen. The heterostructure doped with Fe element, nickel disulfide and bismuth disulfide regulates the electronic structure and valence state of nickel, has an interface effect, regulates the charge distribution of the nickel, obviously improves the electrocatalytic oxygen evolution performance of the nickel, and has good stability. The material obtained by the invention has excellent catalytic activity in alkaline oxygen evolution reaction, is simple and easy to obtain, has no toxicity or harm in reaction, is particularly suitable for batch production, and has wide application prospect.
Description
Technical Field
The invention belongs to the technical field of catalysts, and particularly relates to a preparation method and application of an iron-doped coral-shaped heterostructure catalyst.
Background
In the face of exhaustion of fossil energy and severe environmental problems caused by combustion of fossil fuels, scientists are trying to find a new energy source to solve energy and environmental crisis. With the increasing population and the increasing energy demand of developing countries, the transition from single non-renewable fossil energy to multi-energy in the world energy structure is a historical necessity, so that the search for efficient and sustainable renewable clean energy has important strategic significance. The current crisis is solved by urgently finding a proper advanced energy conversion system, and the electrocatalysis is an ideal energy conversion way due to high energy conversion efficiency, easy realization of reaction conditions and selectable reaction. Among them, hydrogen energy is a new energy source which is distinguished in the present research hotspots because of its high energy density and environment-friendly property. The electrocatalytic water decomposition hydrogen production is an environment-friendly and economic hydrogen production mode, and the electrocatalytic water decomposition relates to two catalytic reactions, namely an anode Oxygen Evolution Reaction (OER) and a cathode Hydrogen Evolution Reaction (HER), wherein the oxygen evolution reaction generates oxygen for one section, and the hydrogen evolution reaction generates hydrogen for one section. The high price and low storage capacity of the noble metal oxide of the oxygen evolution catalyst widely used commercially at present hinder further commercial application of hydrogen production by electrocatalytic decomposition of water, so that the search for a catalyst material capable of replacing the noble metal oxide becomes important and difficult for solving the research of oxygen production reaction by electrocatalytic decomposition of water.
At present, some non-metal catalysts have been demonstrated to replace commercial Pt/C for water splitting catalytic reactions. Usually, the electronic regulation of the chemical valence state of the catalyst is carried out by changing the composition structure of the catalyst, or the morphology control is carried out, a heterojunction is constructed or element doping is introduced, the electronic structure of the catalyst can be coordinated, the intrinsic activity of the catalyst is improved, the specific surface area of the catalyst is improved, and more active sites are exposed. However, the existing doping and heterostructure materials still have the problems of low surface activity, low electron transport speed, low hydrogen evolution efficiency and the like, thereby limiting the application. The combined action of doping and a heterostructure can be considered to optimize the electronic structure of the material and provide more active sites, thereby further improving the activity and stability of the oxygen generation reaction by electrolyzing water.
Disclosure of Invention
The invention aims to provide a preparation method of an iron-doped coral-shaped heterostructure catalyst aiming at overcoming the defects of the prior art. The catalyst has a three-dimensional lamellar structure, has high specific surface area and excellent performances such as good conductivity and the like, and can be used for electrocatalytic oxygen evolution reaction.
The purpose of the invention is realized by the following technical scheme: the catalyst successfully realizes the controllable doping of Fe in the Ni3S2/Bi3S2 heterostructure by a one-step hydrothermal method, and synthesizes the catalyst with a three-dimensional lamellar structure. The finally synthesized iron-doped coralliform Ni3S2/Bi3S2 heterostructure catalyst has good conductivity and high specific surface area, exposes more catalytic active sites, and thus has good electrocatalytic oxygen evolution activity and good stability.
A preparation method of an iron-doped coralliform Ni3S2/Bi3S2 heterostructure catalyst comprises the following steps:
(1) Cleaning and drying the foamed nickel for later use;
(2) Putting the foamed nickel obtained in the step (1) into a hydrothermal kettle, uniformly dispersing ferric trichloride hexahydrate, bismuth nitrate pentahydrate and thiourea in ethylene glycol, and transferring the mixture into the hydrothermal kettle to react for 10 to 20 hours at the temperature of between 150 and 180 ℃; the concentration of ferric trichloride hexahydrate in glycol is 0.3-0.5 mg/mL, the concentration of bismuth nitrate pentahydrate in glycol is 4-5 mg/mL, the concentration of thiourea in glycol is 1-1.5 mg/mL, the volume ratio of nickel foam to glycol is 1-5: 10;
(3) And (3) taking out the product obtained in the step (2), sequentially washing the product with water and ethanol, and drying the product in vacuum to obtain the iron-doped coralliform Ni3S2/Bi3S2 heterostructure catalyst.
Further, the concentration of the ferric trichloride hexahydrate in the glycol in the step (2) is 0.33-0.37 mg/mL.
Further, the concentration of the bismuth nitrate pentahydrate in the step (2) in the ethylene glycol is 4-4.5 mg/mL.
Further, the volume ratio of the nickel foam to the ethylene glycol in the step (2) is 1:10.
the invention has the beneficial effects that:
(1) An iron-doped coralliform Ni3S2/Bi3S2 heterostructure electrocatalyst is synthesized by a simple one-step hydrothermal method. The microstructure of the material obtained by the invention is a coralline material formed by combining nanosheet Ni3S2/Bi3S2, the surface is highly wrinkled, a higher specific surface area can be provided in the electrocatalysis process, and compared with the microcosmic shapes such as rodlike shapes, granular shapes and the like in the prior art, more catalytic active sites can be provided, and the kinetics of electrocatalysis oxygen generation is improved. Furthermore, the three-dimensional multilayer structure facilitates oxygen desorption.
(2) Iron doping is introduced while preparing the coralliform Ni3S2/Bi3S 2. Iron doping of the Ni3S2/Bi3S2 heterostructure is realized for the first time under a one-step method, the electronic structure of the material is optimized while the microstructure with high wrinkles is obtained, the electronic transportation capacity of the material is improved, the oxygen evolution reaction barrier is reduced, the generation energy of an intermediate is optimized, and the activity of the oxygen generation reaction of electrolyzed water is greatly improved. In alkaline electrolyte, the current density of 50mA/cm < 2 > overpotential is only 265mV, which is obviously superior to that of undoped Ni3S2/Bi3S2 and Ni3S2.
(3) Has excellent stability. By comparing XRD and SEM before and after reaction, the material has good structural stability, and can still maintain a highly-folded microstructure after reaction, so that the strategy of 'iron doping + heterostructure' in the invention is proved to have excellent electrochemical stability.
(4) The method has the advantages of simple operation, low requirement on equipment, easily obtained used materials, no use of corrosive and polluting solvents, particular suitability for industrial production, high electrochemical oxygen generation activity of the product and wide application prospect. Meanwhile, the scheme can be popularized to the doping preparation of other heterogeneous materials, and has pioneering significance for the development of subsequent electrocatalytic oxygen evolution.
Drawings
FIG. 1 shows X-ray diffraction patterns (XRD) of the material obtained in example 1 before electrochemical reaction (before OER Fe-Ni3S2/Bi3S 2) and after electrochemical reaction (after OER Fe-Ni3S2/Bi3S 2).
FIG. 2 is a Scanning Electron Micrograph (SEM) of the material obtained in example 1 before the electrochemical reaction (before OER Fe-Ni3S2/Bi3S 2) and after the reaction (after OER Fe-Ni3S2/Bi3S 2).
FIG. 3 is a Transmission Electron Micrograph (TEM) of the material obtained in example 1
FIG. 4 shows electrochemical polarization curves of the material (Fe-Ni 3S2/Bi3S 2) obtained in example 1, the sample (Ni 3S2/Bi3S 2) obtained in comparative example 1, and the sample (Ni 3S 2) obtained in comparative example 2 as catalysts for oxygen evolution reaction, respectively.
Detailed Description
The technical solution of the invention is further illustrated below with reference to examples, which are not to be construed as limiting the technical solution.
Example 1:
(1) And 3mL of foamed nickel is sequentially subjected to ultrasonic cleaning in ethanol, water, 3mol/L hydrochloric acid and acetone for 15 minutes and is dried for later use.
(2) And (2) putting the foamed nickel obtained in the step (1) into a hydrothermal kettle, uniformly dispersing 10mg of ferric trichloride hexahydrate, 121.6mg of bismuth nitrate pentahydrate and 33mg of thiourea into 30mL of ethylene glycol, adding into the hydrothermal kettle, and reacting at 160 ℃ for 16 hours.
(3) And (3) taking out the product obtained in the step (2), washing the product with water and ethanol in sequence, and drying the product in vacuum to obtain the iron-doped coral-shaped heterostructure catalyst.
The obtained catalyst is scanned by a CV curve through a traditional three-electrode system, an electrolyte is 1.0mol/L KOH solution, a carbon rod is a counter electrode, a silver chloride electrode is a reference electrode, the iron-doped coralliform Ni3S2/Bi3S2 heterostructure catalyst is prepared into a working electrode with the thickness of 1.5cm multiplied by 1cm, the voltage interval is 0-1V, and the working electrode is washed by ethanol and deionized water after scanning. FIG. 1 is an X-ray diffraction pattern (XRD) of the sample prepared in example 1 before (before OER Fe-Ni3S2/Bi3S 2) and after (after OER Fe-Ni3S2/Bi3S 2) electrochemical reaction, which shows that the material before and after the reaction has significant characteristic peaks of trinickel disulfide and trinickel disulfide, and the peak position and peak intensity have no significant change, thus proving that the electrochemical reaction has little influence on the material itself. FIG. 2 is a Scanning Electron Microscope (SEM) before and after electrochemical reaction of the material prepared in example 1, and it can be found that the material before reaction (before OER Fe-Ni3S2/Bi3S 2) has a coral-like structure and a highly wrinkled surface, while the shape after reaction (after OER Fe-Ni3S2/Bi3S 2) has little change, even exposes more surface area and provides more active sites. FIG. 3 is a Transmission Electron Microscopy (TEM) image of the material obtained in example 1, which can be found to be composed of lamellae of nanometer-scale thickness and width, and is the source of the highly wrinkled microstructure of FIG. 2. FIG. 4 is a graph showing the electrochemical polarization of the material obtained in example 1. Fe-Ni3S2/Bi3S2 as an oxygen evolution reaction catalyst, when the system reached a current density of 50mA/cm2, measured at a sweep rate of 5mV/S, the overpotential was 265mV, which was significantly lower than 290mV for comparative example 1 (Ni 3S2/Bi3S 2) and 400mV for comparative example 2 (Ni 3S 2).
Example 2:
(1) And 3mL of foamed nickel is sequentially subjected to ultrasonic cleaning in ethanol, water, 3mol/L hydrochloric acid and acetone for 15 minutes and is dried for later use.
(2) And (2) putting the foamed nickel obtained in the step (1) into a hydrothermal kettle, uniformly dispersing 9mg of ferric trichloride hexahydrate, 120mg of bismuth nitrate pentahydrate and 45mg of thiourea into 30mL of ethylene glycol, adding into the hydrothermal kettle, and reacting for 16 hours at 160 ℃.
(3) And (3) taking out the product obtained in the step (2), washing the product with water and ethanol in sequence, and drying the product in vacuum to obtain the iron-doped coral-shaped heterostructure catalyst.
The resulting catalyst microscopically appeared as a highly wrinkled coral structure. When used as an electrochemical oxygen evolution electrode, the overpotential was 258mV, significantly lower than 290mV for comparative example 1 (Ni 3S2/Bi3S 2) and 400mV for comparative example 2 (Ni 3S 2), when the system reached a current density of 50mA/cm2, measured at a sweep rate of 5 mV/S.
Example 3:
(1) And 3mL of foamed nickel is sequentially subjected to ultrasonic cleaning in ethanol, water, 3mol/L hydrochloric acid and acetone for 15 minutes and is dried for later use.
(2) And (2) putting the foamed nickel obtained in the step (1) into a hydrothermal kettle, uniformly dispersing 11.1mg of ferric trichloride hexahydrate, 150mg of bismuth nitrate pentahydrate and 36mg of thiourea into 30mL of ethylene glycol, adding into the hydrothermal kettle, and reacting for 20 hours at 150 ℃.
(3) And (3) taking out the product obtained in the step (2), washing the product with water and ethanol in sequence, and drying the product in vacuum to obtain the iron-doped coral-shaped heterostructure catalyst.
The resulting catalyst microscopically appeared as a highly wrinkled coral structure. When used as an electrochemical oxygen evolution electrode, the overpotential was 266mV, significantly lower than 290mV for comparative example 1 (Ni 3S2/Bi3S 2) and 400mV for comparative example 2 (Ni 3S 2), when the system reached a current density of 50mA/cm2, measured at a sweep rate of 5 mV/S.
Example 4:
(1) And 3mL of foamed nickel is sequentially subjected to ultrasonic cleaning in ethanol, water, 3mol/L hydrochloric acid and acetone for 15 minutes and is dried for later use.
(2) And (2) putting the foamed nickel obtained in the step (1) into a hydrothermal kettle, uniformly dispersing 15mg of ferric trichloride hexahydrate, 135mg of bismuth nitrate pentahydrate and 30mg of thiourea into 30mL of ethylene glycol, adding into the hydrothermal kettle, and reacting for 16 hours at 160 ℃.
(3) And (3) taking out the product obtained in the step (2), washing the product with water and ethanol in sequence, and drying the product in vacuum to obtain the iron-doped coral-shaped heterostructure catalyst.
The resulting catalyst microscopically exhibits a highly wrinkled coral-like structure. When used as an electrochemical oxygen evolving electrode, the overpotential when the system reaches a current density of 50mA/cm2, measured at a sweep rate of 5mV/S, is 271mV, which is significantly lower than 290mV for comparative example 1 (Ni 3S2/Bi3S 2) and 400mV for comparative example 2 (Ni 3S 2).
Example 5:
(1) And (3) ultrasonically cleaning 10mL of foamed nickel in ethanol, water, 3mol/L hydrochloric acid and acetone for 15 minutes in sequence, and drying for later use.
(2) And (2) putting the foamed nickel obtained in the step (1) into a hydrothermal kettle, uniformly dispersing 16mg of ferric trichloride hexahydrate, 200mg of bismuth nitrate pentahydrate and 55mg of thiourea into 50mL of ethylene glycol, adding into the hydrothermal kettle, and reacting for 10 hours at 180 ℃.
(3) And (3) taking out the product obtained in the step (2), washing the product with water and ethanol in sequence, and drying the product in vacuum to obtain the iron-doped coral-shaped heterostructure catalyst.
The resulting catalyst microscopically appeared as a highly wrinkled coral structure. When used as an electrochemical oxygen evolution electrode, the overpotential when the system reaches a current density of 50mA/cm2, measured at a sweep rate of 5mV/S, is 269mV, which is significantly lower than 290mV for comparative example 1 (Ni 3S2/Bi3S 2) and 400mV for comparative example 2 (Ni 3S 2).
Comparative example 1: ni3S2/Bi3S2
(1) And 3mL of foamed nickel is sequentially subjected to ultrasonic cleaning in ethanol, water, 3mol/L hydrochloric acid and acetone for 15 minutes and is dried for later use.
(2) And (2) putting the foamed nickel obtained in the step (1) into a hydrothermal kettle, uniformly dispersing 121.6mg of bismuth nitrate pentahydrate and 33mg of thiourea into 30mL of ethylene glycol, adding into the hydrothermal kettle, and reacting at 160 ℃ for 16 hours.
(3) And (3) taking out the product obtained in the step (2), sequentially washing the product with water and ethanol, and drying the product in vacuum to obtain the Ni3S2/Bi3S2 heterostructure catalyst.
Comparative example 2: preparation of Ni3S2
(1) And 3mL of foamed nickel is sequentially subjected to ultrasonic cleaning in ethanol, water, 3mol/L hydrochloric acid and acetone for 15 minutes and is dried for later use.
(2) And (2) putting the foamed nickel obtained in the step (1) into a hydrothermal kettle, uniformly dispersing 33mg of thiourea into 30mL of ethylene glycol, adding into the hydrothermal kettle, and reacting at 160 ℃ for 16 hours.
(3) And (3) taking out the product obtained in the step (2), sequentially washing the product with water and ethanol, and drying the product in vacuum to obtain the Ni3S2/Bi3S2 heterostructure catalyst.
Detailed Description
To further illustrate the technical means and effects of the present invention adopted to achieve the predetermined objects, the following detailed description of the embodiments, structures, features and effects according to the present invention will be made with reference to the accompanying drawings and preferred embodiments.
Although the present invention has been described with reference to the preferred embodiments, it should be understood that various changes, substitutions and alterations can be made herein without departing from the spirit and scope of the invention as defined by the appended claims.
Claims (4)
1. A preparation method of an iron-doped coralliform heterostructure catalyst is characterized by comprising the following steps:
(1) Cleaning and drying the foamed nickel for later use;
(2) Putting the foamed nickel obtained in the step (1) into a hydrothermal kettle, uniformly dispersing ferric trichloride hexahydrate, bismuth nitrate pentahydrate and thiourea in ethylene glycol, and transferring the mixture into the hydrothermal kettle to react for 10 to 20 hours at the temperature of between 150 and 180 ℃; the concentration of ferric trichloride hexahydrate in glycol is 0.3-0.5 mg/mL, the concentration of bismuth nitrate pentahydrate in glycol is 4-5 mg/mL, the concentration of thiourea in glycol is 1-1.5 mg/mL, the volume ratio of nickel foam to glycol is 1-5: 10;
(3) And (3) taking out the product obtained in the step (2), sequentially washing the product with water and ethanol, and drying the product in vacuum to obtain the iron-doped coralliform Ni3S2/Bi3S2 heterostructure catalyst.
2. The method of claim 1, wherein the concentration of ferric chloride hexahydrate in ethylene glycol of step (2) is 0.33-0.37 mg/mL.
3. The method according to claim 1, wherein the concentration of bismuth nitrate pentahydrate in ethylene glycol of step (2) is 4-4.5 mg/mL.
4. The method according to claim 1, wherein the volume ratio of the foamed nickel and the glycol in the step (2) is 1:10.
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Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN111167480A (en) * | 2020-02-14 | 2020-05-19 | 电子科技大学 | Novel oxygen evolution electrocatalyst and preparation method and application thereof |
| CN113106488A (en) * | 2021-03-25 | 2021-07-13 | 中山大学 | Preparation method of iron-doped nickel sulfide oxygen evolution electrocatalyst |
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Patent Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN111167480A (en) * | 2020-02-14 | 2020-05-19 | 电子科技大学 | Novel oxygen evolution electrocatalyst and preparation method and application thereof |
| CN113106488A (en) * | 2021-03-25 | 2021-07-13 | 中山大学 | Preparation method of iron-doped nickel sulfide oxygen evolution electrocatalyst |
Non-Patent Citations (1)
| Title |
|---|
| SHUAI WANG: "Cooperation of iron and bismuth for the synthesis of ternary metal sulfide as self-supporting electrode for enhanced water oxidation", JOURNAL OF ALLOYS AND COMPOUNDS, 19 August 2021 (2021-08-19) * |
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