2.1. Preparation of Pd Electrocatalysts. All chemicals were
of analytical grade and were used as received. The Pd electrocatalysts
were prepared by the pulse microwave-assisted polyol
method as previously described.13 Typically, palladium dichloride
(4.7 mL of 0.1 mol dm-3 PdCl2 solution) was well mixed
with 20 mL of ethylene glycol (EG) in a beaker by stirring in
an ultrasonic bath. XC-72 carbon powders (50.0 mg, Cabot,
USA) were then added into the mixture as the support. As soon
as the pH value of the mixture was adjusted above 10 by the
dropwise addition of 2.0 mol dm-3 NaOH/EG solution, the welldispersed
slurry was obtained after stirring in an ultrasonic bath
for 30 min. Finally, the slurry was dried and heated by an
intermittent microwave heating (IMH) method in a homemade
microwave oven (1000 W, 2.45 GHz) for alternative heat
treatment at 5 s on and 5 s pulse six times. The resulting black
solid sample was filtered, washed, and dried at 80 °C for 10 h
in a vacuum oven.
2.1. Preparation of Pd Electrocatalysts. All chemicals were
of analytical grade and were used as received. The Pd electrocatalysts
were prepared by the pulse microwave-assisted polyol
method as previously described.13 Typically, palladium dichloride
(4.7 mL of 0.1 mol dm-3 PdCl2 solution) was well mixed
with 20 mL of ethylene glycol (EG) in a beaker by stirring in
an ultrasonic bath. XC-72 carbon powders (50.0 mg, Cabot,
USA) were then added into the mixture as the support. As soon
as the pH value of the mixture was adjusted above 10 by the
dropwise addition of 2.0 mol dm-3 NaOH/EG solution, the welldispersed
slurry was obtained after stirring in an ultrasonic bath
for 30 min. Finally, the slurry was dried and heated by an
intermittent microwave heating (IMH) method in a homemade
microwave oven (1000 W, 2.45 GHz) for alternative heat
treatment at 5 s on and 5 s pulse six times. The resulting black
solid sample was filtered, washed, and dried at 80 °C for 10 h
in a vacuum oven.
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