US 12,351,470 B2
Preparation method of graphene-wrapped cobalt Prussian blue nanocrystal composite material and method of preparing working electrode using the same and application thereof
Ying Wang, Shanghai (CN); Fengting Li, Shanghai (CN); and Bincheng Xu, Shanghai (CN)
Assigned to Tongji University, Shanghai (CN)
Filed by Tongji University, Shanghai (CN)
Filed on Sep. 14, 2021, as Appl. No. 17/475,171.
Claims priority of application No. 202110033591.2 (CN), filed on Jan. 12, 2021.
Prior Publication US 2022/0219998 A1, Jul. 14, 2022
Int. Cl. B32B 9/00 (2006.01); C01B 32/198 (2017.01); C01C 3/12 (2006.01); C02F 1/461 (2023.01); C02F 1/467 (2023.01); B82Y 30/00 (2011.01); C02F 101/16 (2006.01)
CPC C01C 3/12 (2013.01) [C01B 32/198 (2017.08); C02F 1/46109 (2013.01); C02F 1/4676 (2013.01); B82Y 30/00 (2013.01); C01P 2004/64 (2013.01); C02F 2001/46138 (2013.01); C02F 2101/163 (2013.01)] 14 Claims
OG exemplary drawing
 
1. A preparation method of a graphene-wrapped cobalt Prussian blue nano-crystalline composite material, comprising the following steps:
(1) adding a ligand solution of 0.1 mol/L-2 mol/L to a graphene oxide solution of 0.1 g/L-10 g/L, stirring the mixed solution for 10 min-60 min and treating the mixed solution ultrasonically for 5 min-30 min to obtain a mixture of a ligand and graphene oxide;
(2) adding a metal salt solution of 0.1 mol/L-2 mol/L to the mixture obtained at step (1), and stirring for 12 h-36 h to obtain a mixture of graphene oxide and cobalt Prussian blue;
(3) centrifuging the mixture obtained at step (2) at a velocity of 10000 rpm-20000 rpm for 10 min-30 min to obtain a solid, and lyophilizing the solid obtained by centrifugation for 24 h-48 h to obtain a graphene oxide supported cobalt Prussian blue nano-crystalline composite;
(4) calcining the graphene oxide supported cobalt Prussian blue nano-crystalline composite obtained at step (3) in an inert atmosphere to obtain the graphene-wrapped cobalt Prussian blue nano-crystalline composite material;
wherein in step (4), a calcination temperature is between about 250° C.-350° C. and a calcination time is between about 1 h-5 h.