Universal preparation and application of nitrogen-rich graphene aerogel loaded monatomic cluster catalyst based on sol-gel method
A technique of graphene airgel and sol-gel method, which is applied to the universal preparation of nitrogen-rich graphene airgel-supported single-atom cluster catalysts, nitrogen-rich graphene airgel-supported single-atom cluster catalysts and its application fields , to achieve the effects of simple and safe operation process, excellent catalytic activity and stability, and good application prospects
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Embodiment 1
[0039] (1) Preparation of g-C 3 N 4 : Put 3g of melamine powder in a porcelain boat, thermally decompose it in Ar gas at 500°C for 2h, and collect g-C after cooling 3 N 4 yellow powder.
[0040] (2) Preparation of GO:
[0041] a) Dissolve 8 mL of concentrated H 2 SO 4 , 1.0g of K 2 S 2 o 8 and 1.0g of P 2 o 5 Mix well in an ice bath, add 3g of graphite powder to the above mixed solution, heat the oil bath to 80°C for pre-oxidation, and keep for 2.5h. Then let stand to cool to room temperature, dilute with 0.5 L of deionized water, collect the solid product by filtration, continue to wash with deionized water until neutral, and dry naturally overnight for use;
[0042] b) Add the solid product prepared in step a) to 120 mL ice-bathed concentrated H 2 SO 4 with concentrated H 3 PO 4 In the mixed concentrated acid (volume ratio is 5:1), then slowly add 12g KMnO 4 , control the temperature below 20°C for further oxidation and keep it for 1h, then raise the temperat...
Embodiment 2
[0047] (1) Preparation of g-C 3 N 4 : Put 5g of melamine powder in a porcelain boat, thermally decompose it in Ar gas at 550°C for 4h, and collect g-C after cooling 3 N 4 yellow powder.
[0048] (2) Preparation of GO:
[0049] a) Dissolve 10 mL of concentrated H 2 SO 4 , 2.0g of K 2 S 2 o 8 and 2.0g of P 2 o 5 Mix well in an ice bath, add 3g of graphite powder to the above mixed solution, heat the oil bath to 80°C for pre-oxidation, and keep for 3h. Then let stand to cool to room temperature, dilute with 0.5 L of deionized water, collect the solid product by filtration, continue to wash with deionized water until neutral, and dry naturally overnight for use;
[0050] b) Add the solid product prepared in step a) to 120 mL ice-bathed concentrated H 2 SO 4 with concentrated H 3 PO 4 In the mixed concentrated acid (volume ratio is 6:1), then slowly add 12g KMnO 4 , control the temperature below 20°C for further oxidation and keep it for 1h, then raise the temperatu...
Embodiment 3
[0059] The nitrogen-rich graphene airgel-supported FeNx single-atom cluster catalyst FeNx-CN / g-GEL prepared in Example 1 and the comparative example were tested for ORR catalytic performance. Test conditions: Weigh 3 mg of catalyst and place it in a 2 mL small test tube, add 975 microliters of isopropanol and 25 microliters of Nafion solution into the upper test tube, and ultrasonicate for 30 minutes; take 15 microliters of slurry and drop it on the surface of the electrode. The ORR performance was tested in 0.1M KOH, the LSV test scan rate was 10mV / s, and the rotation speed was 1600rm. E of FeNx-CN / g-GEL onset It is 1.0V, which is very close to commercial Pt / C (1.04V), and its half-wave potential (E 1 / 2 ) reached 0.90V, 65mV higher than the commercial Pt / C catalyst, and also significantly higher than the half-wave potential of the comparative example (E of CN / g-GEL 1 / 2 is 0.756V, the E of FeNx / g-GEL 1 / 2 is 0.864V).
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