NiFeMoS complex and a preparation method thereof

Abstract

The embodiment of the invention provides a NiFeMoS complex and a preparation method thereof. The preparation method of the NiFeMoS complex comprises the following steps: obtaining a reactant aqueous solution containing nickel salt, iron salt, molybdenum salt and urea; carrying out a hydrothermal reaction on the reactant aqueous solution at the temperature of 150 to 170 DEG C for 8 to 15 hours, andthen performing separation and washing to obtain a complex precursor; calcining and vulcanizing the complex precursor and sulfur powder in inert gas at the temperature of 300 to 600 DEG C for 0.5 to3 hours, wherein the heating rate is 3 to 8 DEG C / min. The NiFeMoS complex prepared by the preparation method provided by the embodiment of the invention has high catalytic performance for hydrogen evolution reactions.

Description

technical field

[0001] The invention relates to the technical field of hydrogen evolution reaction electrocatalysts, in particular to a NiFeMoS composite and a preparation method thereof. Background technique

[0002] Environmental pollution and resource depletion caused by the use of fossil fuels are becoming more and more serious, and people urgently need to develop new energy sources. Hydrogen energy, as a clean and efficient renewable energy, has attracted people's attention. Electrolysis of water is one of the main means of obtaining hydrogen energy, in which a hydrogen evolution reaction (Hydrogen Evolution Reaction, HER) occurs at the cathode. The overpotential of the hydrogen evolution reaction is relatively high, and it is generally necessary to use a noble metal platinum catalyst to reduce the overpotential. However, noble metals are expensive and scarce resources, which limit their application in hydrogen evolution reaction. Therefore, it is necessary to prepar...

Examples

preparation example Construction

[0032] Based on the above-mentioned design idea, the preparation method of the NiFeMoS composite body provided by the present invention includes:

[0033] (1) obtain the reactant aqueous solution containing nickel salt, iron salt, molybdenum salt and urea;

[0034] (2) hydrothermally reacting the reactant aqueous solution at 150-170° C. for 8-15 hours, then separating and washing to obtain a complex precursor;

[0035] (3) Calcining and vulcanizing the composite precursor and sulfur powder in an inert gas, the temperature of calcining and vulcanization is 300-600°C, the time of calcining and vulcanization is 0.5-3 hours, and the heating rate is 3-8°C / min .

[0036] The present invention adopts one-step reaction to obtain MoO 4 2- Intercalated NiFe LDH, the Ni and Fe elements in the laminate are evenly distributed, and evenly distributed iron sulfide (FeS 2 ) and nickel sulfide (NiS 2 or NiS). And the ultra-small molybdenum disulfide nanosheets are obtained through the co...

Embodiment 1

[0053] Weigh 0.556g (2.2mmol) of nickel acetate, 0.202g of ferric nitrate (0.5mmol), 0.6g of urea (10mmol) and 0.5g of ammonium molybdate (0.4mmol), add 40mL of deionized water, and stir for 20 minutes to obtain the reactant aqueous solution;

[0054] The reactant aqueous solution was transferred to a 50mL reaction kettle, and hydrothermal reaction was carried out at 160°C for 10 hours. After the system was cooled to room temperature, it was filtered under reduced pressure, the filter cake (crude product of the complex precursor) was washed three times with deionized water, and the obtained product was vacuum-dried at 50°C. Obtain the composite precursor, referred to as NiFe LDH-MoO 4 .

[0055] Use tube furnace for vulcanization, weigh 0.1g NiFe LDH-MoO 4 and 1g of S powder were respectively placed on both ends of the porcelain boat, wherein the S powder was placed in the upwind place, and calcined at 400°C for 2 hours, the heating rate was 5°C / min, and argon gas was conti...

Embodiment 2

[0057] The NiFeMoS composite was prepared according to the method of Example 1, the difference from Example 1 was that the temperature of calcination and vulcanization was 300° C., and the obtained product was designated as NiFeMoS-300.

technical field

[0001] The invention relates to the technical field of hydrogen evolution reaction electrocatalysts, in particular to a NiFeMoS composite and a preparation method thereof. Background technique

[0002] Environmental pollution and resource depletion caused by the use of fossil fuels are becoming more and more serious, and people urgently need to develop new energy sources. Hydrogen energy, as a clean and efficient renewable energy, has attracted people's attention. Electrolysis of water is one of the main means of obtaining hydrogen energy, in which a hydrogen evolution reaction (Hydrogen Evolution Reaction, HER) occurs at the cathode. The overpotential of the hydrogen evolution reaction is relatively high, and it is generally necessary to use a noble metal platinum catalyst to reduce the overpotential. However, noble metals are expensive and scarce resources, which limit their application in hydrogen evolution reaction. Therefore, it is necessary to prepar...

Examples

preparation example Construction

[0032] Based on the above-mentioned design idea, the preparation method of the NiFeMoS composite body provided by the present invention includes:

[0033] (1) obtain the reactant aqueous solution containing nickel salt, iron salt, molybdenum salt and urea;

[0034] (2) hydrothermally reacting the reactant aqueous solution at 150-170° C. for 8-15 hours, then separating and washing to obtain a complex precursor;

[0035] (3) Calcining and vulcanizing the composite precursor and sulfur powder in an inert gas, the temperature of calcining and vulcanization is 300-600°C, the time of calcining and vulcanization is 0.5-3 hours, and the heating rate is 3-8°C / min .

[0036] The present invention adopts one-step reaction to obtain MoO 4 2- Intercalated NiFe LDH, the Ni and Fe elements in the laminate are evenly distributed, and evenly distributed iron sulfide (FeS 2 ) and nickel sulfide (NiS 2 or NiS). And the ultra-small molybdenum disulfide nanosheets are obtained through the co...

Embodiment 1

[0053] Weigh 0.556g (2.2mmol) of nickel acetate, 0.202g of ferric nitrate (0.5mmol), 0.6g of urea (10mmol) and 0.5g of ammonium molybdate (0.4mmol), add 40mL of deionized water, and stir for 20 minutes to obtain the reactant aqueous solution;

[0054] The reactant aqueous solution was transferred to a 50mL reaction kettle, and hydrothermal reaction was carried out at 160°C for 10 hours. After the system was cooled to room temperature, it was filtered under reduced pressure, the filter cake (crude product of the complex precursor) was washed three times with deionized water, and the obtained product was vacuum-dried at 50°C. Obtain the composite precursor, referred to as NiFe LDH-MoO 4 .

[0055] Use tube furnace for vulcanization, weigh 0.1g NiFe LDH-MoO 4 and 1g of S powder were respectively placed on both ends of the porcelain boat, wherein the S powder was placed in the upwind place, and calcined at 400°C for 2 hours, the heating rate was 5°C / min, and argon gas was conti...

Embodiment 2

[0057] The NiFeMoS composite was prepared according to the method of Example 1, the difference from Example 1 was that the temperature of calcination and vulcanization was 300° C., and the obtained product was designated as NiFeMoS-300.

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