CN114411195A - Nickel manganese selenide heterojunction electrocatalyst and preparation method and application thereof - Google Patents
Nickel manganese selenide heterojunction electrocatalyst and preparation method and application thereof Download PDFInfo
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- CN114411195A CN114411195A CN202210032249.5A CN202210032249A CN114411195A CN 114411195 A CN114411195 A CN 114411195A CN 202210032249 A CN202210032249 A CN 202210032249A CN 114411195 A CN114411195 A CN 114411195A
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Abstract
The invention relates to a nickel manganese selenide heterojunction electrocatalyst and a preparation method and application thereof, wherein the preparation method of the electrocatalyst comprises the following steps: 1) dissolving nickel salt and manganese salt in deionized water, adding potassium persulfate, immersing carbon cloth with a clean surface in the obtained mixed solution, dripping weak alkaline solution, and growing on the carbon cloth to obtain a layered nickel-manganese hydroxide nanosheet; 2) calcining the carbon cloth for the first time to obtain a precursor nickel-manganese oxide; 3) and (3) arranging carbon at the downstream of the tubular furnace, arranging selenium powder at the upstream of the tubular furnace, and carrying out secondary calcination to obtain the nickel-manganese selenide heterojunction electrocatalyst. The nickel manganese selenide heterojunction electrocatalyst provided by the invention has excellent electrochemical activity, and HER reaches 10mA cm‑2The current density of the electrode only needs 158mV overpotential, and the OER reaches 50mAcm‑2The current density of the electrolytic water only needs 422mV overpotential, and the electrolytic water has high efficiency and good cycle stability.
Description
Technical Field
The invention belongs to the technical field of production of hydrogen or hydrogen-containing mixed gas, and particularly relates to a nickel manganese selenide heterojunction electrocatalyst, and a preparation method and application thereof.
Background
The hydrogen produced by electrolyzing water is a current green hydrogen production method due to simple process and mature technology, and has attracted much attention in recent years. The Hydrogen Evolution Reaction (HER) at the cathode and the Oxygen Evolution Reaction (OER) at the anode play an important role in the electrolytic conversion of water into hydrogen. The overpotential required by the reaction can be effectively reduced under the action of the electrocatalyst, so that the hydrogen production efficiency is improved. The common catalyst of HER and OER is composed of noble metals of platinum, iridium, ruthenium and alloy and compound thereof, but the high cost and natural scarcity hinder the wider application thereof, in recent years, with the development of the field of electrocatalysis, the appearance of transition metal chalcogenide, nitride, carbide and phosphide brings new opportunities for the field, but the existing electrocatalysis still has the problems of low catalytic activity, poor stability, short service life and the like, and the development of hydrogen production by water electrolysis is hindered.
Disclosure of Invention
The technical problem to be solved by the invention is to provide a nickel manganese selenide heterojunction electrocatalyst, a preparation method and an application thereof aiming at the defects in the prior art, wherein the nickel manganese selenide heterojunction electrocatalyst has better stability and long service life under the condition of high current density.
In order to solve the technical problems, the technical scheme provided by the invention is as follows:
a nickel manganese selenide heterojunction electrocatalyst is prepared by the following specific steps:
1) dissolving nickel salt and manganese salt in deionized water, adding potassium persulfate to obtain a mixed solution, immersing carbon cloth with a clean surface in the mixed solution, dropwise adding a weak alkaline solution into the mixed solution while stirring, standing for 20-30 min after dropwise adding is finished, and growing on the carbon cloth to obtain a layered nickel-manganese hydroxide nanosheet;
2) placing the carbon cloth with the layered nickel-manganese hydroxide nanosheets grown on the surface in the step 1) in a porcelain boat, placing the porcelain boat in a tube furnace for primary calcination, and obtaining a precursor nickel-manganese oxide on the surface of the carbon cloth;
3) and (3) arranging the carbon coated with the precursor nickel manganese oxide on the surface in the step 2) at the downstream of the tubular furnace, arranging selenium powder at the upstream of the tubular furnace, setting different temperatures at the upstream and the downstream, introducing hydrogen, allowing the hydrogen to flow through the downstream from the upstream of the tubular furnace, and performing secondary calcination to obtain the nickel manganese selenide heterojunction electrocatalyst.
According to the scheme, the nickel salt in the step 1) is one of nickel nitrate, nickel chloride, nickel phosphide, nickel bromide and nickel sulfate.
According to the scheme, the manganese salt in the step 1) is one of manganese sulfate, manganese nitrate, manganese acetate and manganese chloride; the molar ratio of the nickel salt to the manganese salt is 1: 1 to 4.
According to the scheme, the concentration of potassium persulfate in the mixed solution in the step 1) is 0.005-0.015 mol/L. The potassium persulfate is used as a hydrothermal auxiliary agent to promote the growth of the nickel-manganese hydroxide on the carbon cloth.
According to the scheme, the concentration of nickel ions in the mixed solution in the step 1) is 0.2-0.3 mol/L, and the concentration of manganese ions is 0.2-1.2 mol/L.
According to the scheme, the weak alkaline solution in the step 1) is one of ammonia water solution, sodium bicarbonate solution and potassium bicarbonate solution, the pH value is 7-10, and the volume ratio of the weak alkaline solution to the mixed solution is 0.01-0.03: 1. the alkalescent solution provides hydroxide radicals to generate nickel-manganese hydroxide on the surface of the carbon cloth.
According to the scheme, the first calcination process conditions in the step 2) are as follows: heating to 200-600 ℃ at room temperature at a heating rate of 3-8 ℃/min, and preserving heat for 20-30 min.
According to the scheme, the mass ratio of the selenium powder in the step 3) to the mass of the carbon cloth coated with the precursor nickel manganese oxide is 1: 1 to 2.
According to the scheme, in the second calcination process in the step 3), the upstream temperature of the tubular furnace is 300-400 ℃, the downstream temperature is 400-500 ℃, and the calcination time is 1-3 hours.
The invention also comprises a preparation method of the nickel manganese selenide heterojunction electrocatalyst, which comprises the following specific steps:
4) dissolving nickel salt and manganese salt in deionized water, adding potassium persulfate to obtain a mixed solution, immersing carbon cloth with a clean surface in the mixed solution, dropwise adding a weak alkaline solution into the mixed solution while stirring, standing for 20-30 min after dropwise adding is finished, and growing on the carbon cloth to obtain a layered nickel-manganese hydroxide nanosheet;
5) placing the carbon cloth with the layered nickel-manganese hydroxide nanosheets grown on the surface in the step 1) in a porcelain boat, placing the porcelain boat in a tube furnace for primary calcination, and obtaining a precursor nickel-manganese oxide on the surface of the carbon cloth;
6) and (3) arranging the carbon coated with the precursor nickel manganese oxide on the surface in the step 2) at the downstream of the tubular furnace, arranging selenium powder at the upstream of the tubular furnace, setting different temperatures at the upstream and the downstream, introducing hydrogen, allowing the hydrogen to flow through the downstream from the upstream of the tubular furnace, and performing secondary calcination to obtain the nickel manganese selenide heterojunction electrocatalyst.
The invention also comprises the application of the nickel manganese selenide heterojunction electrocatalyst in the aspect of hydrogen production by water electrolysis.
The nickel manganese selenide heterojunction electrocatalyst provided by the invention is a two-dimensional layered structure, has a stable structure, selenium element has a wide electronic regulation range, the selenium-based heterostructure has excellent catalytic performance in hydrogen evolution and oxygen evolution, and the heterostructure in the material increases the lattice distortion degree, so that the catalytic activity is enhanced, and the heterostructure material has a plurality of active sites and uniform component distribution, and has the advantages of better electrolytic water catalytic performance.
The invention has the beneficial effects that: 1. the nickel manganese selenide heterojunction electrocatalyst provided by the invention has excellent electrochemical activity, and HER reaches 10mA cm-2The current density of the electrode only needs 158mV overpotential, and the OER reaches 50mAcm-2The current density of the electrolytic water only needs 422mV overpotential, and the electrolytic water has high efficiency and good cycle stability. 2. The preparation method has the advantages of fewer process steps, lower calcination temperature, less energy consumption and low cost.
Drawings
FIG. 1 is an XRD pattern of a nickel manganese selenide heterojunction electrocatalyst prepared in example 1 of the present invention;
FIG. 2 is an OER performance test plot of the nickel manganese selenide heterojunction electrocatalyst prepared in example 1 and the nickel manganese oxide precursor before selenization in 1M KOH;
fig. 3 is a HER performance test plot in 1M KOH for the nickel manganese selenide heterojunction electrocatalyst prepared in example 1.
Detailed Description
In order to make the technical solutions of the present invention better understood, the present invention is further described in detail below with reference to the accompanying drawings.
Example 1
A nickel manganese selenide heterojunction electrocatalyst is prepared by the following specific steps:
dissolving 0.08mol of nickel chloride, 0.08mol of manganese nitrate and 0.003mol of potassium persulfate in 300mL of deionized water, stirring for 10min to obtain a mixed solution, and mixing 9cm of the mixed solution2Adding carbon cloth (pre-placed in deionized water for ultrasonic treatment to remove surface grease and impurities) into the mixed solution, stirring for 3min, then dropwise adding 4mL of ammonia water solution with the pH value of 8 into the solution while stirring at 15 ℃, standing for 20min after dropwise adding, taking out, drying, placing into a tubular furnace, heating to 300 ℃ from room temperature at the heating rate of 5 ℃/min, preserving heat for 30min to obtain carbon cloth (500mg) coated with nickel-manganese oxide layered nanosheets, washing the prepared carbon cloth coated with nickel-manganese oxide layered nanosheets for 3-5 times by deionized water and alcohol, placing into a 60 ℃ blast drying oven for drying, then placing into the downstream of a double-temperature-zone tubular furnace, placing 400mg of selenium powder into the upstream of the tubular furnace, introducing hydrogen, allowing the hydrogen to flow from the upstream to the downstream of the tubular furnace, setting the upstream temperature of the tubular furnace to be 320 ℃, setting the downstream temperature to be 420 ℃, reacting for 1h to obtain the nickel manganese selenide heterojunction electrocatalyst.
As shown in fig. 1, which is an XRD pattern of the nickel manganese selenide heterojunction electrocatalyst prepared in this example, XRD test results show that there are nickel selenide manganese selenide crystals in the electrocatalyst.
The product was subjected to a Linear Sweep Voltammetry (LSV) test, performed on an electrochemical workstation of CHI660e, using three electrodesA polar system is tested, the nickel manganese selenide heterojunction electrocatalyst electrode prepared in the embodiment is a working electrode, Hg/HgO is a reference electrode, a graphite rod is a counter electrode, an electrolyte is 1M KOH, and the sweep rate of the polarization curve test of HER and OER is 5mV s-1. The conversion formula between the applied voltage and the reversible hydrogen electrode is ERHE＝EHg/HgO+0.0591pH+0.098。
FIG. 2 shows the OER polarization curve of the nickel manganese selenide heterojunction electrocatalyst prepared in the embodiment tested by a three-electrode system in 1M KOH, the test voltage range is 1-2V (relative to a standard hydrogen electrode), the OER theoretical potential is 1.23V, the working electrode generates oxygen evolution reaction, and when the OER reaches 50mAcm-2The current density of the nickel manganese selenide heterojunction electrocatalyst prepared in the embodiment is only 422mV of overpotential, which is lower than that of a nickel manganese oxide precursor before selenization (a carbon cloth coated by the nickel manganese oxide layered nanosheet prepared in the embodiment, which is cut into 0.36cm of carbon cloth2) The overpotential of (c).
FIG. 3 shows the HER polarization curve of the nickel manganese selenide heterojunction electrocatalyst prepared in the embodiment measured by a three-electrode system in 1M KOH, the test voltage range is 0-0.5V (relative to a standard hydrogen electrode), the HER theoretical potential is 0V, the working electrode generates oxygen evolution reaction, and when the HER reaches 10mAcm-2The nickel manganese selenide heterojunction electrocatalyst prepared in this example requires only 158mV of overpotential.
The results of the above LSV tests demonstrate that the electrocatalysts prepared in this example perform well.
Example 2
A nickel manganese selenide heterojunction electrocatalyst is prepared by the following specific steps:
dissolving 0.08mol of nickel chloride, 0.16mol of manganese nitrate and 0.003mol of potassium persulfate in 300mL of deionized water, stirring for 10min to obtain a mixed solution, and performing ultrasonic treatment to remove 9cm of surface grease and impurities2Adding carbon cloth into the mixed solution, stirring for 3min, adding dropwise 4mL of ammonia water solution with pH value of 9 into the solution at 15 deg.C under stirring, standing for 20min, drying, heating to 350 deg.C at 5 deg.C/min, and maintaining the temperature for 30 deg.CAnd min, obtaining carbon cloth (700mg) coated by the nickel manganese oxide layered nanosheets, washing the prepared carbon cloth coated by the nickel manganese oxide layered nanosheets for 3-5 times by using deionized water and alcohol, drying the carbon cloth in a 60 ℃ blast drying box, then placing the carbon cloth at the downstream of a tubular furnace with two temperature zones, placing 600mg of selenium powder at the upstream of the tubular furnace, introducing hydrogen, enabling the hydrogen to flow through the downstream from the upstream of the tubular furnace, setting the upstream temperature of the tubular furnace to be 340 ℃, setting the downstream temperature to be 440 ℃, and reacting for 2 hours to obtain the nickel manganese selenide heterojunction electrocatalyst.
Example 3
A nickel manganese selenide heterojunction electrocatalyst is prepared by the following specific steps:
dissolving 0.08mol of nickel chloride, 0.32mol of manganese nitrate and 0.003mol of potassium persulfate in 300mL of deionized water, stirring for 10min to obtain a mixed solution, and performing ultrasonic treatment to remove 9cm of surface grease and impurities2Adding carbon cloth into the mixed solution, stirring for 3min, then dropwise adding 4mL of ammonia water solution with the pH value of 8 into the solution while stirring at 15 ℃, standing for 20min after dropwise adding, taking out after drying, putting into a tubular furnace, heating to 400 ℃ from room temperature at the heating rate of 5 ℃/min, keeping the temperature for 30min to obtain carbon cloth (600mg) coated with nickel-manganese oxide layered nanosheets, washing the prepared carbon cloth coated with the nickel-manganese oxide layered nanosheets for 3-5 times by deionized water and alcohol, putting into a blast drying box at 60 ℃, drying, then putting into the downstream of the tubular furnace with a double temperature zone, putting 500mg of selenium powder into the upstream of the tubular furnace, introducing hydrogen, allowing the hydrogen to flow through the downstream from the upstream of the tubular furnace, setting the upstream temperature of the tubular furnace to be 360 ℃, setting the downstream temperature to be 460 ℃, and reacting for 3h to obtain the nickel-manganese selenide heterojunction electrocatalyst.
Claims (10)
1. The nickel manganese selenide heterojunction electrocatalyst is characterized in that the preparation method comprises the following specific steps:
1) dissolving nickel salt and manganese salt in deionized water, adding potassium persulfate to obtain a mixed solution, immersing carbon cloth with a clean surface in the mixed solution, dropwise adding a weak alkaline solution into the mixed solution while stirring, standing for 20-30 min after dropwise adding is finished, and growing on the carbon cloth to obtain a layered nickel-manganese hydroxide nanosheet;
2) placing the carbon cloth with the layered nickel-manganese hydroxide nanosheets grown on the surface in the step 1) in a porcelain boat, placing the porcelain boat in a tube furnace for primary calcination, and obtaining a precursor nickel-manganese oxide on the surface of the carbon cloth;
3) and (3) arranging the carbon coated with the precursor nickel manganese oxide on the surface in the step 2) at the downstream of the tubular furnace, arranging selenium powder at the upstream of the tubular furnace, setting different temperatures at the upstream and the downstream, introducing hydrogen, allowing the hydrogen to flow through the downstream from the upstream of the tubular furnace, and performing secondary calcination to obtain the nickel manganese selenide heterojunction electrocatalyst.
2. The nickel manganese selenide heterojunction electrocatalyst according to claim 1, wherein the nickel salt in step 1) is one of nickel nitrate, nickel chloride, nickel phosphide, nickel bromide, nickel sulfate; the manganese salt is one of manganese sulfate, manganese nitrate, manganese acetate and manganese chloride; the molar ratio of the nickel salt to the manganese salt is 1: 1 to 4.
3. The nickel manganese selenide heterojunction electrocatalyst according to claim 1, wherein the concentration of potassium persulfate in the mixed solution of step 1) is 0.005-0.015 mol/L.
4. The nickel manganese selenide heterojunction electrocatalyst according to claim 1, wherein the concentration of nickel ions in the mixed solution in step 1) is 0.2 to 0.3mol/L, and the concentration of manganese ions is 0.2 to 1.2 mol/L.
5. The nickel manganese selenide heterojunction electrocatalyst according to claim 1, wherein the weak alkaline solution in step 1) is one of an ammonia solution, a sodium bicarbonate solution and a potassium bicarbonate solution, the pH value of the weak alkaline solution is 7 to 10, the volume ratio of the weak alkaline solution to the mixed solution is 0.01 to 0.03: 1.
6. the nickel manganese selenide heterojunction electrocatalyst according to claim 1, wherein the first calcination process conditions in step 2) are: heating to 200-600 ℃ at room temperature at a heating rate of 3-8 ℃/min, and preserving heat for 20-30 min.
7. The nickel manganese selenide heterojunction electrocatalyst according to claim 1, wherein the mass ratio of the selenium powder in step 3) to the mass of the carbon cloth coated with the precursor nickel manganese oxide on the surface is 1: 1 to 2.
8. The nickel manganese selenide heterojunction electrocatalyst according to claim 1, wherein in the second calcination process in step 3), the upstream temperature of the tube furnace is 300-400 ℃, the downstream temperature is 400-500 ℃, and the calcination time is 1-3 h.
9. A method for preparing a nickel manganese selenide heterojunction electrocatalyst according to any one of claims 1 to 8, characterized by comprising the following specific steps:
1) dissolving nickel salt and manganese salt in deionized water, adding potassium persulfate to obtain a mixed solution, immersing carbon cloth with a clean surface in the mixed solution, dropwise adding a weak alkaline solution into the mixed solution while stirring, standing for 20-30 min after dropwise adding is finished, and growing on the carbon cloth to obtain a layered nickel-manganese hydroxide nanosheet;
2) placing the carbon cloth with the layered nickel-manganese hydroxide nanosheets grown on the surface in the step 1) in a porcelain boat, placing the porcelain boat in a tube furnace for primary calcination, and obtaining a precursor nickel-manganese oxide on the surface of the carbon cloth;
3) and (3) arranging the carbon coated with the precursor nickel manganese oxide on the surface in the step 2) at the downstream of the tubular furnace, arranging selenium powder at the upstream of the tubular furnace, setting different temperatures at the upstream and the downstream, introducing hydrogen, allowing the hydrogen to flow through the downstream from the upstream of the tubular furnace, and performing secondary calcination to obtain the nickel manganese selenide heterojunction electrocatalyst.
10. Use of a nickel manganese selenide heterojunction electrocatalyst according to any one of claims 1 to 8 in the production of hydrogen by electrolysis of water.
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| CN115011989A (en) * | 2022-05-31 | 2022-09-06 | 武汉工程大学 | Nickel-manganese nitride catalyst and preparation method and application thereof |
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