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Rotating Disk Slurry Au Electrodeposition at Unsupported Carbon Vulcan XC-72 and Ce3+ Impregnation for Ethanol Oxidation in Alkaline Media

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Abstract

A robust electrodeposition method consisting of the rotating disk slurry electrode (RoDSE) technique to obtain Au nanoparticles highly dispersed on a conductive carbonaceous support, i.e., Vulcan XC-72R, for ethanol electrooxidation reaction in alkaline media was developed. Ceria was used as a cocatalyst using a Ce(III)-EDTA impregnation method in order to enhance the catalytic activity and improve the catalyst’s overall stability. The RoDSE method used to obtain highly dispersed Au nanoparticles does not require the use of a reducing agent or stabilizing agent, and the noble-metal loading was controlled by the addition and tuning of the metal precursor concentration. Inductively coupled plasma and thermogravimetric analysis indicated that the Au loading in the catalyst was 9 %. Particle size and characteristic Au fcc crystal facets were determined by X-ray diffraction. The morphology of the catalyst was also investigated using electron microscopy techniques. In addition, X-ray absorption spectroscopy was used to corroborate the presence and identify the oxidation state of Ce in the system and to observe if there are any electronic interactions within the 8 % Au/CeOx/C system. Cyclic voltammetry of electrodeposited 9 % Au/C and Ce-promoted 8 % Au/C showed a higher catalytic current density for ethanol oxidation when compared with commercially available catalysts (20 % Au/C) of a higher precious metal loading. In addition, we report a higher stability toward the ethanol electrooxidation process, which was corroborated by 1 mV/s linear sweep voltammetry and chronoamperometric studies.

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Acknowledgements

We would like to thank NASA-MIRO Center of Advanced Nanoscale Materials Grant Number NNX10AQ17A and NASA-EPSCoR Grant Number NNX14AN18A for the financial support of this research project. Use of the National Synchrotron Light Source, Brookhaven National Laboratory, was supported by the U.S. Department of Energy, Office of Science, Office of Basic Energy Sciences, under Contract No. DE-AC02-98CH10886. The authors would also like to acknowledge Prof. Eduardo Nicolau (UPR), Dr. Steven N. Ehrlich (NSLS), Dr. Syed Khalid (NSLS), and Dr. Nebojša Marinković (NSLS) for their help with experimental setup at Beamline X-18A. LEB was a NSF-LSAMP Bridge-to the-Doctorate Fellow (NSF Grant CMMI 1025020).

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Correspondence to Carlos R. Cabrera.

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Betancourt, L.E., Guzmán-Blas, R., Luo, S. et al. Rotating Disk Slurry Au Electrodeposition at Unsupported Carbon Vulcan XC-72 and Ce3+ Impregnation for Ethanol Oxidation in Alkaline Media. Electrocatalysis 8, 87–94 (2017). https://doi.org/10.1007/s12678-016-0342-x

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