The electrochemical reduction of
highly oxidized unsupported graphene oxide nanosheets and its platinum
electrodeposition was done by the rotating disk slurry electrode technique.
Avoiding the use of a solid electrode, graphene oxide was electrochemically
reduced in a slurry solution with a scalable process without the use
of a reducing agent. Graphene oxide nanosheets were synthesized from
carbon platelet nanofibers to obtain highly hydrophilic layers of
less than 250 nm in width. The graphene oxide and electrochemically
reduced graphene oxide/Pt (erGOx/Pt) hybrid materials were characterized
through different spectroscopy and microscopy techniques. Pt nanoparticles
with 100 facets, clusters, and atoms at erGOx were identified by high
resolution transmission electron microscopy (HRTEM). Cyclic voltammetry
was used to characterize the electrocatalytic activity of the highly
dispersed erGOx/Pt hybrid material toward the oxidation of ammonia,
which showed a 5-fold current density increase when compared with
commercially available Vulcan/Pt 20%. This is in agreement with having
Pt (100) facets present in the HRTEM images of the erGOx/Pt material.
The Rotating Disk Slurry Electrodeposition (RoDSE) technique is a novel method allowing to deposit electrochemically metal nanoparticles on a given conductive support and produce a powder catalyst for diverse applications, for example, ethanol oxidation reaction (EOR). This technique was used to electrodeposit Pd nanoparticles on carbon Vulcan XC-72R nanoflakes at three different applied potentials (0.0, 0.4, and 0.7 V vs. RHE). The potentials were chosen based on different regions of Pd electrodeposition on a clean glassy carbon electrode. Each Pd/Vulcan catalyst was characterized through different spectroscopic, microscopic, and electrochemical techniques. Powder X-ray diffraction and transmission electron microscopy studies verified the Pd crystallinity and particle size, respectively. The Pd particle size decreased with a more positive applied electrodeposition potential at carbon Vulcan XC-72R nanoflakes. X-ray photoelectron spectroscopy determined that the applied potential affected, both, the final palladium and carbon oxidation states. Finally, cyclic voltammetry was used to characterize the electrocatalytic activity of each Pd / Vulcan catalyst in 0.1M KOH and for the EOR. It was found that, for Pd electrodeposition, an applied potential of 0.4 V vs. RHE provided harmony between a mass transport and kinetically controlled deposition thereby providing the optimal conditions to produce a better catalyst with better EOR.
Enantioselective metalations are comparatively rare. The three‐membered ring (–)‐(2) has been produced in 12% optical yield by this method. Thermal rearrangement of this methyleneaziridine to the cyclopropanimine (3) is stereospecific.
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