US 12,103,087 B2
Systems and methods for platinum nanocatalyst synthesis via continuous flow reactor
Rongyue Wang, Naperville, IL (US); Krzysztof Z. Pupek, Plainfield, IL (US); Vojislav Stamenkovic, Naperville, IL (US); and Trevor L. Dzwiniel, Carol Stream, IL (US)
Assigned to UChicago Argonne, LLC, Chicago, IL (US)
Filed by UCHICAGO ARGONNE, LLC, Chicago, IL (US)
Filed on Sep. 30, 2019, as Appl. No. 16/587,507.
Prior Publication US 2021/0094024 A1, Apr. 1, 2021
Int. Cl. B01J 23/89 (2006.01); B22F 9/24 (2006.01); B22F 1/054 (2022.01); B82Y 30/00 (2011.01)
CPC B22F 9/24 (2013.01) [B01J 23/892 (2013.01); B22F 1/054 (2022.01); B22F 2301/25 (2013.01); B22F 2998/10 (2013.01); B82Y 30/00 (2013.01)] 16 Claims
OG exemplary drawing
 
1. A method of synthesizing Pt nanoparticle catalyst comprising the steps of:
forming, at an initial temperature of 18-28° C., a reaction mixture comprising a metal precursor comprising nickel acetate tetrahydrate, a reducing agent comprising 1,2-tetradecanediol, and a surfactant comprising one part oleic acid to two parts oleylamine, a platinum precursor comprising platinum acetylacetonate, and a polar solvent;
heating the reaction mixture at 110° C. for two hours, removing water;
injecting a segment of reaction mixture into a continuous flow reactor at a temperature of at least 190° C. for 5 minutes to 1 hour, forming a PtNi nanoparticle solution, the segment having a segment length of at least 3 mm;
isolating PtNi/substrate nanoparticles by:
sonicating the PtNi nanoparticle solution with substrate in chloroform solution,
adding hexane to the sonicated chloroform solution,
precipitating PtNi/substrate nanoparticles, and
collecting the PtNi/substrate nanoparticles by filtration;
annealing the PtNi/substrate nanoparticles in air at a first annealing temperature, removing surfactant from the PtNi/substrate nanoparticles;
acid leaching the PtNi/substrate nanoparticles by:
sonicating the collected PtNi/substrate nanoparticles in water,
mixing an acid with the sonicated PtNi/substrate sonicated in water for 60 minutes to form leached PtNi/substrate nanoparticles, and
collecting the leached PtNi/substrate nanoparticles by filtration; and
annealing the leached PtNi/substrate nanoparticles at a second annealing temperature, forming a Pt-skin on the PtNi/substrate nanoparticles.