A method for synthesizing a foamed nickel loaded iron nickel phosphorus C3N4 electrocatalytic material

Abstract

The application discloses a synthesis method of a foamed nickel loaded iron-nickel-phosphorus C3N4 electrocatalytic material, and specifically comprises the following steps: S1, potassium ferricyanide, citric acid and C3N4 are weighed respectively and added into deionized water, and magnetic stirring is performed through a magnetic stirrer until complete dissolution; S2, 2cm*2cm foamed nickel is cut, surface impurities are washed away, and the treated foamed nickel is dried in a vacuum oven at 70 DEG C for 6h, and the dried foamed nickel is placed in the solution prepared in S1, and the reactor is sealed; S3, the foamed nickel in S2 is dried in a vacuum oven at 70 DEG C for 12h, is placed in the upstream of a porcelain boat, 450mg-550mg sodium hypophosphite is weighed and placed in the downstream of the porcelain boat, the porcelain boat is placed in the middle position of a tube furnace, and the foamed nickel is subjected to phosphating reaction in an argon atmosphere, the reaction temperature is controlled to be 345-355 DEG C, the reaction time is controlled to be 115-125min, and the foamed nickel loaded iron-nickel-phosphorus / C3N4 electrocatalytic material is obtained after the reaction is completed. The foamed nickel surface participates in the formation of a metal organic compound, so that the performance of the material is improved, and the service life of the material is prolonged.

Description

Technical Field

[0001] This invention relates to the field of materials synthesis, specifically to a method for synthesizing a nickel-foamed nickel-phosphorus C3N4 electrocatalytic material. Background Technology

[0002] With the increasing popularity of zinc-air batteries, their cathode catalysts have become a research hotspot. Prussian blue and its analogues have attracted widespread attention due to their open-framework structure, which provides abundant three-dimensional diffusion channels. However, Prussian blue has poor electrical conductivity, resulting in slow electron transfer, and it undergoes structural collapse and aggregation under gas erosion. Therefore, it cannot be used directly as an electrocatalyst, but rather as a precursor for obtaining better-performing catalysts through subsequent treatments such as phosphating, sulfidation, and nitriding.

[0003] Nickel foam possesses excellent electrical conductivity, a large specific surface area, and a porous structure. As a porous metallic material, nickel foam is widely used as a current collector and catalyst support in chemical power sources and water electrolysis devices. Generally, nickel foam-supported electrodes are obtained through two methods: one is to coat a pre-prepared electrode active material onto the surface of the nickel foam; the other is to use the surface of the nickel foam as the site for preparing the electrode active material, which grows simultaneously with the formation of the active material on the surface of the nickel foam. Both methods result in nickel foam-supported electrodes exhibiting problems such as active material clogging the pores of the nickel foam, weak contact between the active material and the surface of the nickel foam, and easy detachment of the active material. Therefore, a method for synthesizing a nickel foam-supported iron-nickel-phosphorus C3N4 electrocatalytic material is provided. Summary of the Invention

[0004] The purpose of this invention is to address the deficiencies of the prior art by providing a method for synthesizing nickel-iron-phosphorus C3N4 electrocatalytic materials supported on nickel foam, thereby solving the problems mentioned in the background art.

[0005] To achieve the above objectives, the present invention provides the following technical solution: a method for synthesizing a nickel-foamed nickel-phosphorus C3N4 electrocatalytic material, the specific steps of which are as follows:

[0006] S1: Weigh out potassium ferricyanide, citric acid, and C3N4 respectively and add them to deionized water. Stir with a magnetic stirrer until completely dissolved.

[0007] S2: Cut a 2cm*2cm piece of nickel foam, wash away surface impurities, place the treated nickel foam in a vacuum oven at 70℃ for 6 hours, place the dried nickel foam in the solution prepared in S1, and seal the reactor.

[0008] S3: Dry the nickel foam from S2 in a vacuum oven at 70°C for 12 hours, place it upstream of a ceramic boat, weigh 450mg-550mg of sodium hypophosphite and place it downstream of the ceramic boat, place the ceramic boat in the middle of a tube furnace, and allow the nickel foam to undergo a phosphating reaction in an argon atmosphere. Control the reaction temperature at 345-355°C and the reaction time at 115-125 minutes. After the reaction is complete, the nickel foam-supported iron-nickel-phosphorus / C3N4 electrocatalytic material is obtained.

[0009] As a preferred embodiment of the present invention, the potassium ferricyanide weighed in S1 is 320-340 mg, citric acid is 180-200 mg, C3N4 is 85-95 mg, and deionized water is 15 ml.

[0010] As a preferred embodiment of the present invention, the rotation speed of the magnetic stirrer in S1 is 1000 r / min.

[0011] As a preferred embodiment of the present invention, in step S2, the dried nickel foam is placed in the solution prepared in step S1, the reactor is sealed, and the reaction temperature is controlled at 95-105°C and the reaction time is 175-185 min.

[0012] As a preferred technical solution of the present invention, the method for washing the foamed nickel in S2 is as follows: first, ultrasonic treatment with 3 mol / L hydrochloric acid for 15 minutes, then ultrasonic treatment with deionized water for 15 minutes, and finally ultrasonic treatment with ethanol.

[0013] The beneficial effects of this invention are: the nickel foam surface of this method participates in the formation of organometallic compounds, thereby improving the performance of the synthesized material and increasing its service life. Attached Figure Description

[0014] Figure 1 This is one of the 500-micrometer SEM images of this invention;

[0015] Figure 2 This is the second 500-micrometer SEM image of the present invention;

[0016] Figure 3 The XRD pattern of this invention;

[0017] Figure 4 This is the OER test diagram of the present invention;

[0018] Figure 5 This is a test diagram for the present invention. Detailed Implementation

[0019] The preferred embodiments of the present invention will now be described in detail with reference to the accompanying drawings, so that the advantages and features of the present invention can be more easily understood by those skilled in the art, thereby providing a clearer and more explicit definition of the scope of protection of the present invention.

[0020] Example: According to Figure 1-5 This invention provides a technical solution: a method for synthesizing a nickel-foamed nickel-phosphorus C3N4 electrocatalytic material, the specific steps of which are as follows:

[0021] S1: Weigh out 320-340 mg of potassium ferricyanide, 180-200 mg of citric acid, and 85-95 mg of C3N4 and add them to 15 ml of deionized water. Stir magnetically until completely dissolved. The speed of the magnetic stirrer is 1000 r / min.

[0022] S2: Cut 2cm*2cm pieces of nickel foam, wash away surface impurities, and the washing method is as follows: first, sonicate with 3 mol / L hydrochloric acid for 15 minutes, then sonicate with deionized water for 15 minutes, and finally sonicate with ethanol. Place the treated nickel foam in a vacuum oven at 70℃ for 6 hours to dry. Place the dried nickel foam in the solution prepared in S1, seal the reactor, and control the reaction temperature at 95-105℃ for 175-185 minutes.

[0023] S3: Dry the nickel foam from S2 in a vacuum oven at 70°C for 12 hours, place it upstream of a ceramic boat, weigh 450mg-550mg of sodium hypophosphite and place it downstream of the ceramic boat, place the ceramic boat in the middle of a tube furnace, and allow the nickel foam to undergo a phosphating reaction in an argon atmosphere. Control the reaction temperature at 345-355°C and the reaction time at 115-125 minutes. After the reaction is complete, the nickel foam-supported iron-nickel-phosphorus / C3N4 electrocatalytic material is obtained.

[0024] In this method, the surface of the foamed nickel participates in the formation of organometallic compounds, thereby improving the performance of the synthesized material and extending its service life.

[0025] The above embodiments merely illustrate several implementation methods of the present invention, and their descriptions are relatively specific and detailed, but they should not be construed as limiting the scope of the invention patent. It should be noted that those skilled in the art can make various modifications and improvements without departing from the concept of the present invention, and these all fall within the protection scope of the present invention.

Claims

1. A method for synthesizing a nickel-foamed nickel-phosphorus C3N4 electrocatalytic material, characterized in that: The specific steps are as follows: S1: Weigh out potassium ferricyanide, citric acid, and C3N4 separately and add them to deionized water. Stir with a magnetic stirrer until completely dissolved. The amount of potassium ferricyanide is 320-340 mg, citric acid is 180-200 mg, C3N4 is 85-95 mg, and deionized water is 15 ml. S2: Cut a 2cm*2cm piece of nickel foam, wash away surface impurities, and dry the treated nickel foam in a vacuum oven at 70℃ for 6 hours. Place the dried nickel foam in the solution prepared in S1 and seal the reactor. The washing method for nickel foam is as follows: first, sonicate with 3 mol / L hydrochloric acid for 15 minutes, then sonicate with deionized water for 15 minutes, and finally sonicate with ethanol. S3: Dry the nickel foam from S2 in a vacuum oven at 70°C for 12 hours, place it upstream of a ceramic boat, weigh 450mg-550mg of sodium hypophosphite and place it downstream of the ceramic boat, place the ceramic boat in the middle of a tube furnace, and allow the nickel foam to undergo a phosphating reaction in an argon atmosphere. Control the reaction temperature at 345-355°C and the reaction time at 115-125 minutes. After the reaction is complete, the nickel foam-supported iron-nickel-phosphorus / C3N4 electrocatalytic material is obtained.

2. The method for synthesizing a nickel-foamed supported iron-nickel-phosphorus C3N4 electrocatalytic material according to claim 1, characterized in that: The magnetic stirrer in S1 rotates at a speed of 1000 r / min.

3. The method for synthesizing a nickel-foamed supported iron-nickel-phosphorus C3N4 electrocatalytic material according to claim 1, characterized in that: In step S2, the dried nickel foam is placed in the solution prepared in step S1, the reactor is sealed, and the reaction temperature is controlled at 95-105℃ for 175-185 min.

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