CN113443610B - Ruthenium selenide nanosphere electrocatalyst and preparation method and application thereof - Google Patents

Ruthenium selenide nanosphere electrocatalyst and preparation method and application thereof Download PDF

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CN113443610B
CN113443610B CN202110779961.7A CN202110779961A CN113443610B CN 113443610 B CN113443610 B CN 113443610B CN 202110779961 A CN202110779961 A CN 202110779961A CN 113443610 B CN113443610 B CN 113443610B
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ruse
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ruthenium
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CN113443610A (en
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马江权
詹伟
李楠
李正萍
郭志敏
强成宏
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Changzhou University
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    • C—CHEMISTRY; METALLURGY
    • C01—INORGANIC CHEMISTRY
    • C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
    • C01B19/00—Selenium; Tellurium; Compounds thereof
    • C01B19/007—Tellurides or selenides of metals
    • 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
    • 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
    • C25B11/00—Electrodes; Manufacture thereof not otherwise provided for
    • C25B11/04—Electrodes; Manufacture thereof not otherwise provided for characterised by the material
    • C25B11/051—Electrodes formed of electrocatalysts on a substrate or carrier
    • C25B11/073—Electrodes formed of electrocatalysts on a substrate or carrier characterised by the electrocatalyst material
    • C25B11/075—Electrodes formed of electrocatalysts on a substrate or carrier characterised by the electrocatalyst material consisting of a single catalytic element or catalytic compound
    • C—CHEMISTRY; METALLURGY
    • C01—INORGANIC CHEMISTRY
    • C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
    • C01P2002/00—Crystal-structural characteristics
    • C01P2002/70—Crystal-structural characteristics defined by measured X-ray, neutron or electron diffraction data
    • C01P2002/72—Crystal-structural characteristics defined by measured X-ray, neutron or electron diffraction data by d-values or two theta-values, e.g. as X-ray diagram
    • C—CHEMISTRY; METALLURGY
    • C01—INORGANIC CHEMISTRY
    • C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
    • C01P2004/00—Particle morphology
    • C01P2004/01—Particle morphology depicted by an image
    • C01P2004/03—Particle morphology depicted by an image obtained by SEM
    • C—CHEMISTRY; METALLURGY
    • C01—INORGANIC CHEMISTRY
    • C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
    • C01P2004/00—Particle morphology
    • C01P2004/30—Particle morphology extending in three dimensions
    • C01P2004/32—Spheres
    • C—CHEMISTRY; METALLURGY
    • C01—INORGANIC CHEMISTRY
    • C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
    • C01P2004/00—Particle morphology
    • C01P2004/60—Particles characterised by their size
    • C01P2004/62—Submicrometer sized, i.e. from 0.1-1 micrometer
    • 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 belongs to the field of electrocatalyst preparation and application, and in particular relates to a ruthenium selenide nanosphere electrocatalyst, a preparation method and application thereof, wherein a ruthenium selenide precursor is prepared by utilizing a microwave synthesis method, and RuSe is obtained after further calcining by a tube furnace 2 The nanosphere electrocatalyst has excellent hydrogen evolution performance in KOH, which is close to the performance of noble metal Pt/C catalysts. The invention provides a method for preparing RuSe by adopting a microwave and calcination two-step method 2 The nanosphere electrocatalyst has the advantages of short synthesis time, simple operation, greenness and no pollution, and the catalyst has excellent hydrogen evolution activity and good stability in electrocatalysis.

Description

Ruthenium selenide nanosphere electrocatalyst and preparation method and application thereof
Technical Field
The invention belongs to the field of electrocatalyst preparation and application, and in particular relates to a ruthenium selenide nanosphere electrocatalyst and a preparation method and application thereof.
Background
Hydrogen fuel is considered a promising candidate for solving the global environment and energy crisis because of its renewable, no greenhouse gas emissions, and highest energy density among all fuels. Currently, a widely used method of hydrogen fuel production is steam reforming of fossil fuels, but this process produces emissions of carbon dioxide and air pollutants. Electrochemical water splitting hydrogen production has received increasing attention in recent years as an advanced clean energy conversion technology. The key of this technology is the two half reactions of cathodic Hydrogen Evolution Reaction (HER) and anodic Oxygen Evolution Reaction (OER), which produce H separately 2 And O 2 And (3) gas.
In alkaline electrolytes, the HER process is not only dependent on H 2 Adsorption kinetics of O, also dependent on H 2 Dissociation rate of O. Ru is a noble metal catalyst, but its price is far lower than Pt, and Ru has good water dissociation energy, and the hydrogen bond strength is almost equivalent to Pt. However, ru metals exhibit high oxygen affinity, resulting in adsorption of oxygen-containing species (OH:)Strong and cause the active sites in the subsequent hydrogen evolution process to be vacated too slowly, thereby impeding the overall hydrogen evolution process.
Disclosure of Invention
The invention aims to provide a RuSe 2 The nanosphere electrocatalyst and the preparation method thereof are applied to prepare hydrogen by decomposing water under alkaline conditions, and have high catalytic activity and good stability.
The technical scheme of the invention is as follows: the invention provides a RuSe 2 The preparation method of the nanosphere electrocatalyst comprises the following steps: ruCl is to be processed 3 The aqueous solution and selenium source were dispersed in ethylene glycol and stirred thoroughly. Placing the dispersion liquid into a microwave reactor for microwave reaction, centrifugally washing and vacuum drying the obtained precipitate, and further calcining in a tube furnace to obtain crystal RuSe 2 Nanosphere electrocatalyst.
The specific technical process is as follows:
(1) An amount of Se powder or H 2 SeO 3 As a selenium source, dissolved in ethylene glycol, and thoroughly stirred until it is completely dispersed. Wherein Se powder or H 2 SeO 3 The molar ratio of the catalyst to the glycol is as follows: 1:1000-1:5000.
As preferable: 50ml of ethylene glycol was weighed by the measuring cylinder, poured into a beaker, and 0.0311g of Se powder was added thereto, followed by stirring for 1 hour.
(2) A certain amount of RuCl 3 Slowly adding the mixture into the dispersion liquid in the step (1), stirring and carrying out ultrasonic treatment until the mixture is uniformly dispersed, and regulating the pH value of the solution to be alkaline by using KOH. Wherein RuCl is added 3 With Se powder or H 2 SeO 3 The molar ratio of (2) is: 1:1-1:3, and adjusting the pH range of the solution to be: 6 to 10.
As preferable: weigh 0.0181g RuCl 3 Slowly adding the mixture into the beaker filled with the dispersion liquid in the step (1), stirring and dispersing for 1h, uniformly dispersing by ultrasonic for 1h, and adjusting the pH of the solution to be 8 by using a KOH solution with the concentration of 0.1mol/L to be alkaline.
(3) And (3) reacting the dispersion liquid obtained in the step (2) in a rapid microwave reactor at a certain temperature for a certain time, cooling the solution after the reaction to room temperature, centrifugally washing and drying in vacuum.
Wherein, the power of the rapid microwave reactor is as follows: 600W-1000W, the reaction time in the rapid microwave reactor is as follows: 2 min-6 min.
As preferable: placing the beaker with the dispersion liquid in the step (2) in a microwave reactor, setting the power of the microwave reactor to 800W, the reaction time to 3 minutes, cooling to room temperature after the reaction is finished, centrifugally washing the suspension liquid containing the product for 5-6 times to remove residual glycol, and placing the product in a vacuum drying oven at 60 ℃ for overnight to obtain the product RuSe 2 A precursor.
(4) The product RuSe obtained in the step (3) is processed 2 The precursor is arranged in N 2 Calcining in an atmosphere tube furnace at different time and temperature to obtain the final product crystal RuSe 2 Nanosphere electrocatalyst.
The calcination temperature in the tube furnace is: the calcination time is 200-600 ℃, and the calcination time is as follows: and 1-4 h.
As preferable: the product RuSe in the step (3) is processed 2 The precursor is placed in a crucible, and the crucible is placed in N 2 Setting and controlling the heating rate to be 5 ℃/min, the calcining temperature to be 500 ℃ and the calcining time to be 2h in an atmosphere tube furnace, and obtaining the final product crystal RuSe after the calcining is completed 2 A nanosphere.
The invention selects proper selenium source, controls Se powder and RuCl 3 Is prepared through microwave synthesis of RuSe by microwave method under the conditions of proportion and microwave reaction time 2 Precursor, and then changing different calcining temperatures and times to prepare crystal RuSe 2 A nanosphere. Through controlling the calcination temperature and time, ruSe with higher crystallization degree and regular morphology can be obtained 2 The nanosphere electrocatalyst enables the composite electrocatalyst to have high catalytic activity and good stability in electrocatalytic hydrogen evolution reaction.
The invention also provides a RuSe 2 The nanosphere electrocatalyst is used as a working electrode for preparing hydrogen by electrolyzing water under alkaline conditions.
Electrocatalyst RuSe prepared by microwave and calcination two-step method 2 The nanosphere is applied to an electrocatalytic hydrogen evolution performance test method, a three-electrode system is used, and a working electrode is loaded with RuSe 2 The counter electrode is stoneThe ink stick electrode, the reference electrode is Hg/HgO electrode, and the electrolyte is 1mol/L KOH solution.
The invention has the technical effects that:
(1) The invention provides a method for preparing crystalline RuSe by utilizing microwave and calcination two-step method 2 Compared with the traditional hydrothermal method and the like, the nanospheres have the characteristics of novel synthesis method, simple conditions, easiness in operation, rapidness, high efficiency, energy conservation, environmental protection, easiness in industrial production and the like;
(2) The invention provides a method for preparing RuSe by utilizing microwave 2 The precursor has good crystallinity and regular morphology after the calcination temperature and time are controlled, so that the electrochemical active surface area is increased, and the precursor has high activity and good stability for electrocatalytic hydrogen evolution reaction;
(3) The invention provides a method for preparing crystalline RuSe by utilizing microwave and calcination two-step method 2 Nanospheres have high catalytic hydrogen evolution activity and good stability in alkaline electrolyte, and hydrogen is prepared by electrocatalytically decomposing water in KOH electrolyte with concentration of 1mol/L, so as to obtain calcined crystal RuSe 2 The nanospheres are working electrodes, and the current density is-10 mA/cm 2 When the overpotential is only 29mV, the catalyst has excellent catalytic performance and stability for electrolytic water hydrogen evolution reaction.
Drawings
FIG. 1 shows the crystalline RuSe obtained in example 1 of the present invention 2 SEM image of nanospheres.
FIG. 2 is a crystalline RuSe obtained in example 2 of the present invention 2 SEM image of nanospheres.
FIG. 3 is a crystalline RuSe obtained in example 3 of the present invention 2 SEM image of nanospheres.
FIG. 4 is a crystalline RuSe obtained in example 4 of the present invention 2 SEM image of nanospheres.
FIG. 5 is a crystalline RuSe obtained in example 5 of the present invention 2 SEM image of nanospheres.
FIG. 6 is a crystalline RuSe obtained in comparative example 2 of the present invention 2 SEM image of nanospheres.
FIG. 7 shows the crystalline RuSe obtained in examples 1 to 5 of the present invention 2 XRD pattern of nanospheres.
FIG. 8 shows the crystalline RuSe obtained in examples 1 to 5 of the present invention 2 Polarization profile of nanospheres electrolyzed water HER in 1.0M KOH solution.
FIG. 9 shows the crystalline RuSe obtained in examples 1 to 5 of the present invention 2 Tafel plot of nanospheres electrolyzed water HER in 1.0M KOH solution.
FIG. 10 is a crystalline RuSe obtained in example 1 of the present invention 2 Polarization curves (built-in graph is crystal RuSe obtained in the example) of nanospheres obtained before and after 1000 circles of cyclic voltammetry scanning test 2 Current time profile of nanospheres for 17 hours of electrolysis of water at an overpotential of 29 mV).
Detailed Description
The technical features of the present invention will be further illustrated by the following examples, but the scope of the present invention is not limited to the following examples.
Example 1
Preparation of Se powder Dispersion
50ml of ethylene glycol was weighed by the measuring cylinder, poured into a beaker, and 0.0311g of Se powder was added thereto, followed by stirring for 1 hour.
Preparation of 2.1mol/L KOH solution
50mL of ultrapure water, 5.61g of potassium hydroxide was weighed, dissolved and stirred with ultrapure water, and after cooling, the volume was determined in a 100mL volumetric flask.
Se powder dispersion and RuCl 3 Preparation of the Mixed solution
Accurately weigh 0.0181g RuCl 3 Slowly adding into a beaker filled with Se dispersion, stirring and dispersing for 1h, uniformly dispersing by ultrasonic for 1h, and adjusting to be alkaline by using KOH solution with the concentration of 0.1mol/L to ensure that the pH value of the solution is=8.
4.RuSe 2 Preparation of nanospheres
(1) Placing the beaker with the dispersion liquid in a microwave reactor, setting the power of the microwave reactor at 800W for 3min, cooling to room temperature after the reaction is finished, centrifugally washing the suspension liquid containing the product for 5 times to remove residual glycol, and placing the product in a vacuum drying oven at 60 ℃ for overnight to obtain the product RuSe 2 A precursor.
(2) RuSe is to 2 Placing the precursor in a crucible, and placing the cruciblePut in N 2 Setting and controlling the heating rate to be 5 ℃/min, the calcining temperature to be 500 ℃ and the calcining time to be 2h in an atmosphere tube furnace, and obtaining the final product crystal RuSe after the calcining is completed 2 A nanosphere.
Crystalline RuSe prepared in example 1 2 As can be seen from the SEM image shown in FIG. 1 and the XRD image shown in FIG. 7, the prepared RuSe is 2 The characteristic peak of the nanometer ball XRD is sharp and obvious, and is the same as the standard card RuSe 2 Completely accords with the regular sphere shape with uniform morphology, and the prepared crystal RuSe 2 The nanospheres have good crystallinity and regular morphology.
Example 2
Compared with example 1, the difference is that: in RuSe 2 In the preparation step (2) of the nanospheres, the calcination temperature was set to 200 ℃, and other preparation methods were the same as in example 1. As can be seen from XRD and scanning electron microscope images, the prepared RuSe 2 And RuSe 2 The precursor has similar characteristic peaks, mainly the characteristic peaks of Se powder, but the product morphology is not regular and uniform enough.
Example 3
Compared with example 1, the difference is that: in RuSe 2 In the preparation step (2) of the nanospheres, the calcination temperature was set to 300 ℃, and other preparation methods were the same as in example 1. As can be seen from XRD and scanning electron microscope images, the prepared RuSe 2 And RuSe 2 The characteristic peak is obviously changed compared with the precursor, compared with RuSe 2 The characteristic peaks of the standard card completely correspond to each other, but the crystallinity of the product is still not high, and the appearance is regular spheroid.
Example 4
Compared with example 1, the difference is that: in RuSe 2 In the preparation step (2) of the nanospheres, the calcination temperature was set at 400 ℃, and other preparation methods were the same as in example 1. As can be seen from XRD and scanning electron microscope images, the prepared RuSe 2 The characteristic peak is more obvious, the crystallinity of the product is also higher, and the appearance is in a more uniform regular sphere shape.
Example 5
Compared with example 1, the difference is that: in RuSe 2 Preparation of nanospheres(2) The calcination temperature was set at 600℃and the other preparation methods were the same as in example 1. As can be seen from XRD and scanning electron microscope images, the prepared RuSe 2 The characteristic peak is sharper and more obvious, the crystallinity of the product is higher, and the appearance is uniform regular sphere.
Example 6
Compared with example 1, the difference is that: ruCl 3 And Se powder in a molar ratio of 1:3, and the other preparation methods are the same as in example 1.
Example 7
Compared with example 1, the difference is that: ruCl 3 And Se powder in a molar ratio of 1:1, and the other preparation methods are the same as in example 1.
Example 8
Compared with example 1, the difference is that: changing Se powder into 0.0508 and 0.0508g H 2 SeO 3 Other preparation methods were the same as in example 1.
Example 9
Compared with example 1, the difference is that: the molar ratio of Se powder to glycol is as follows: 1:5000, other preparation methods are the same as in example 1.
Comparative example 1
Compared with example 1, the difference is that: the procedure of example 1 was followed except that deionized water was used as the reaction solvent instead of ethylene glycol. When ionized water is used as a reaction solvent instead of ethylene glycol, the reactant Se powder cannot be completely dispersed and dissolved, and the reaction is not sufficiently complete.
Comparative example 2
Compared with example 1, the difference is that: not subjected to RuSe 2 Preparation of nanospheres calcination step in step (2), other preparation methods were as in example 1. As can be seen from XRD and scanning electron microscope images, the prepared RuSe 2 The characteristic peak of the precursor XRD is mainly the characteristic peak of Se powder, and the product has poor crystallinity and irregular and uniform morphology.
The ratio of the raw materials used, the reaction conditions, and the prepared electrocatalyst of the above examples and comparative examples gave an anode having a current density of 10mA/cm 2 The overpotential at this time is shown in Table 1.
TABLE 1
Application example 1
1. Activation treatment of electrocatalyst
(1) Catalyst ink was prepared by dispersing 2mg of catalyst and 10. Mu.L of 5wt% Nafion in a mixed solution containing 375. Mu.L of ultrapure water and 125. Mu.L of ethanol. After continuing the ultrasonic treatment for 20 minutes, 5. Mu.L of uniform ink was dropped on a pre-polished 3mm diameter glassy carbon electrode, followed by natural drying at room temperature.
(2) The working electrode was surface-coated with the crystalline RuSe of example 1 using a three electrode system 2 The glassy carbon electrode of (2) is a graphite rod electrode, the reference electrode is an Hg/HgO electrode, and the electrolyte is 1mol/L KOH;
(3) Cyclic Voltammetry (CV) activation: the electrochemical workstation of Shanghai Chenhua DH7000 is used, a CV program is adopted, the test interval is between-0.8 and-1.6V vs. RHE, the sweeping speed is 50mV/s, the cycle is 20, and the electrode reaches a stable state.
2. Linear Sweep Voltammetry (LSV) test
After activation, the switching procedure was a linear sweep voltammetry procedure with a test interval of-0.8 to-1.6V vs. RHE, a sweep rate of 5mV/s, and an electrocatalyst in alkaline electrolyte at-10 mA/cm 2 At this time, the overpotential was 29mV, as shown in FIG. 8.
3. Stability test
After activation, the switching procedure was a chronoamperometric procedure, with a voltage set of 29mv and a time set of 61200s. As shown in fig. 10, the voltage of the electrocatalyst does not change much, demonstrating its good stability.
Application example 2
As shown in application example 1, ruSe prepared in example 2 2 The electrocatalyst is used for preparing hydrogen by the electrocatalytic decomposition of water in KOH electrolyte with the concentration of 1mol/L, and the anode has the current density of 10mA/cm 2 At this time, the overpotential was 86mV for the electrocatalyst.
Application example 3
As shown in application example 1, ruSe prepared in example 3 2 The electrocatalyst is used for preparing hydrogen by the electrocatalytic decomposition of water in KOH electrolyte with the concentration of 1mol/L, and the anode has the current density of 10mA/cm 2 At this time, the overpotential was 68mV for the electrocatalyst.
Application example 4
As shown in application example 1, ruSe prepared in example 4 2 The electrocatalyst is used for preparing hydrogen by the electrocatalytic decomposition of water in KOH electrolyte with the concentration of 1mol/L, and the anode has the current density of 10mA/cm 2 At this time, the overpotential was 49mV for the electrocatalyst.
Application example 5
As shown in application example 1, ruSe prepared in example 5 2 The electrocatalyst is used for preparing hydrogen by the electrocatalytic decomposition of water in KOH electrolyte with the concentration of 1mol/L, and the anode has the current density of 10mA/cm 2 At this time, the overpotential was 39mV for the electrocatalyst.
Application example 6
As shown in application example 1, ruSe prepared in example 6 2 The electrocatalyst is used for preparing hydrogen by the electrocatalytic decomposition of water in KOH electrolyte with the concentration of 1mol/L, and the anode has the current density of 10mA/cm 2 At this time, the overpotential was 48mV for the electrocatalyst.
Application example 7
As shown in application example 1, ruSe prepared in example 7 2 The electrocatalyst is used for preparing hydrogen by the electrocatalytic decomposition of water in KOH electrolyte with the concentration of 1mol/L, and the anode has the current density of 10mA/cm 2 At this time, the overpotential was 40mV for the electrocatalyst.
Application example 8
As shown in application example 1, ruSe prepared in example 8 2 The electrocatalyst is used for preparing hydrogen by the electrocatalytic decomposition of water in KOH electrolyte with the concentration of 1mol/L, and the anode has the current density of 10mA/cm 2 At this time, the overpotential was 51mV for the electrocatalyst.
Application example 9
As shown in application example 1, ruSe prepared in example 9 2 The electrocatalyst is used for preparing hydrogen by the electrocatalytic decomposition of water in KOH electrolyte with the concentration of 1mol/L, and the anode has the current density of 10mA/cm 2 At this time, the overpotential was 45mV for the electrocatalyst.
Application example 10
As shown in application example 1, ruSe prepared in comparative example 1 2 The electrocatalyst is used for preparing hydrogen by the electrocatalytic decomposition of water in KOH electrolyte with the concentration of 1mol/L, and the anode has the current density of 10mA/cm 2 At this time, the overpotential was 146mV for the electrocatalyst.
Application example 11
As shown in application example 1, ruSe prepared in comparative example 2 2 The electrocatalyst is used for preparing hydrogen by the electrocatalytic decomposition of water in KOH electrolyte with the concentration of 1mol/L, and the anode has the current density of 10mA/cm 2 At this time, the overpotential was 109mV for the electrocatalyst.
The foregoing detailed description of the preferred embodiments and advantages of the invention will be appreciated that the foregoing description is merely illustrative of the presently preferred embodiments of the invention, and that no changes, additions, substitutions and equivalents of those embodiments are intended to be included within the scope of the invention.

Claims (4)

1. The ruthenium selenide nanosphere electrocatalyst for electrocatalytic hydrogen evolution under alkaline condition is characterized in that the ruthenium selenide nanosphere electrocatalyst is RuSe with regular morphology and high crystallinity 2 A nanosphere;
the preparation method of the ruthenium selenide nanosphere electrocatalyst comprises the following specific steps:
(1) By mixing Se powder or H 2 SeO 3 Dissolving in glycol as selenium source, stirring thoroughly until it is completely dispersed;
(2) RuCl is to be processed 3 Slowly adding the mixture into the dispersion liquid obtained in the step (1), stirring the mixture by ultrasonic until the mixture is uniformly dispersed, and regulating the pH value of the solution to be alkaline by using KOH;
(3) Reacting the dispersion liquid obtained in the step (2) in a rapid microwave reactor with the power of 800W for 3min, cooling the obtained product to room temperature, centrifugally washing and drying in vacuum;
(4) Placing the product obtained in the step (3) in N 2 Calcining in an atmosphere tube furnace to obtain a final product crystal RuSe 2 Nanosphere electrocatalyst;
the calcination temperature is as follows: the calcination time is 200-600 ℃, and the calcination time is as follows: and 1-4 hours.
2. Ruthenium selenide nanosphere electrocatalyst according to claim 1, wherein in step (1) Se powder or H 2 SeO 3 The molar ratio of the catalyst to the glycol is as follows: 1:1000-1:5000.
3. The ruthenium selenide nanosphere electrocatalyst according to claim 1, wherein the RuCl added in step (2) 3 With Se powder or H 2 SeO 3 The molar ratio of (2) is: 1:1 to 1:3.
4. The ruthenium selenide nanospheres electrocatalyst according to claim 1, wherein the pH of the solution is adjusted in step (2) to: 6-10.
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CN111939940A (en) * 2020-07-03 2020-11-17 南方科技大学 Ruthenium-based catalyst and preparation method and application thereof

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CN111715245A (en) * 2019-03-21 2020-09-29 扬州大学 Based on high catalytic activity and crystalline RuTe2The electrolytic water catalyst and the preparation method thereof
CN111939940A (en) * 2020-07-03 2020-11-17 南方科技大学 Ruthenium-based catalyst and preparation method and application thereof

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