Method for producing carbon-supported Pt shell-core catalyst by means of liquid phase reduction of H2
A catalyst and reducing agent technology, applied in the field of preparation of high-performance low-Pt shell-core catalysts, can solve the problems of insufficient activity, stability, loading, and cost, and achieve high-efficiency oxygen reduction activity, good activity and stability, and catalysts. low load effect
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Embodiment 1
[0045] Take PVP (polyvinylpyrrolidone) 0.057g and dissolve it in a mixed solution of 50mL ethanol and 30mL water, add 0.1M CuCl 2 Solution 2mL, add carbon carrier XC-72 50mg, ultrasonic dispersion 30min. in N 2 Under protection, in an oil bath at 80°C, add 0.03g of alkaline reducing agent NaBH4, including 0.015g of NaOH, 30mL of water, N 2 Protected at 80°C and stirred for 1h. Add 0.015mol / L H 2 PtCl 6 Solution 3mL,N 2 Under protection, replace for 2h. Added oxalate chelated MoCl 5 (0.02g) and H 2 PtCl 6 (0.015mol / L, 3mL) mixed solution, adjust pH=11, in H 2 Under reducing conditions, react at 80°C for 4h to prepare the alloy shell structure. Add NaBH 4 0.2g, NaOH0.06g, in N 2 The crystals were aged overnight under protection. Centrifuge and dry at 60°C to obtain a highly active low-platinum Pt alloy core-shell catalyst.
Embodiment 2
[0047] Take PVP (polyvinylpyrrolidone) 0.057g and dissolve it in a mixed solution of 50mL ethanol and 30mL water, add 0.1M CuCl 2 Solution 2mL, add carbon carrier XC-72 50mg, ultrasonic dispersion 30min. in N 2 Under protection, 80°C oil bath, add alkaline reducing agent NaBH 4 0.03g, of which NaOH 0.015g, water 30mL, N 2 Protected at 80°C and stirred for 1h. Add 0.015mol / L H 2 PtCl 6 Solution 3mL,N 2 Under protection, replace for 2h. Added oxalate chelated MoCl 5 (0.02g) and H 2 PtCl 6(0.015mol / L, 3mL) mixed solution, adjust pH=5, in H 2 Under reducing conditions, react at 80°C for 4h to prepare the alloy shell structure. Add NaBH 4 0.2g, NaOH 0.06g, in N 2 The crystals were aged overnight under protection. Centrifuge and dry at 60°C to obtain a highly active low-platinum Pt alloy core-shell catalyst.
Embodiment 3
[0049] Electrochemical tests were performed in a three-electrode system to characterize the oxygen reduction activity of the catalysts. The electrolyte solution of this system is 0.1mol L -1 HClO 4 , the counter electrode is a Pt sheet electrode, the reference electrode is a saturated calomel electrode, and the cyclic voltammetry test electrolyte solution is N 2 Saturation, the test system is Gamry3000; ORR test solution is O 2 saturation. Preparation of the catalytic layer of the rotating disk electrode membrane: 40% Pt / C catalyst: 5mg catalyst, 2.5mL isopropanol, ultrasonication; add 50 μL of 5wt% Nafion solution, ultrasonication, take 3.2 μL of the above dispersed slurry and coat it on a rotating disk electrode The disc electrode surface, as the working electrode. Due to the low loading of Cu@PtMo / C catalyst, preparation of membrane catalyst layer: 5mg catalyst, 2.5mL isopropanol, ultrasonication; add 50μL of 5wt% Nafion solution, ultrasonication, take 8μL of the above ...
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