Preparation of High Surface Area Cu-Au Bimetallic Nanostructured Materials by Co-electrodeposition in a Deep Eutectic Solvent
Elena Plaza-Mayoral a, Paula Sebastian-Pascual a, Kim Nicole Dalby b, Kim Degn Jensen a, Ib Chorkendorff c, Hanne Falsig b, Maria Escudero-Escribano a
a Department of Chemistry, Center for High Entropy Alloy Catalysis, University of Copenhagen, Universitetsparken, 5, København, Denmark
b Haldor Topsøe A/S, Haldor Topsøes Allé, 1, Kongens Lyngby, Denmark
c Department of Physics, Surface Physics and Catalysis, Technical University of Denmark, Fysikvej, DK-2800 Lyngby, Denmark
Proceedings of nanoGe Fall Meeting 2021 (NFM21)
#SolFuel21. Solar Fuel: In-situ and operando characterization of electrified interfaces
Online, Spain, 2021 October 18th - 22nd
Organizers: Bastian Mei, Jan Philipp Hofmann and María Escudero-Escribano
Poster, Elena Plaza-Mayoral, 284
Publication date: 23rd September 2021

Developing new inexpensive strategies for controlled preparation of nanostructured materials in an environmentally friendly manner is crucial to move towards a sustainable industry. To fill this purpose, electrodeposition in green deep eutectic solvents (DES) has been proposed as a sustainable alternative for the synthesis of bimetallic nanostructures with high active surface area. Herein, we present the preparation of Cu-Au bimetallic high active area nanostructures with tunable structure and composition. Cu-Au systems have been widely explored due to its potential for different reactions such as CO2 reduction.

In this work, we have investigated the effect of the applied potential and bath composition, containing the metal salt precursors, in the electrodeposition of Cu-Au bimetallic nanostructures in chlorine chloride plus urea DES. Cyclic voltammograms and chronoamperometric curves were recorded to assess the co-deposition mechanism and to establish the optimal potential conditions for the preparation of the bimetallic films. Ex-situ field emission scanning electron microscopy (FE-SEM), electron dispersive spectroscopy (EDS) and X-ray photoelectron microscopy (XPS) were combined to examine the morphology, chemical composition and distribution of Au and Cu in the nanostructured deposits. Tailored morphology and composition were obtained by specifically tuning the applied potential conditions and concentration of salt precursors in the DES. Finally, we estimate the increase of the electroactive surface area through the analysis of the lead underpotential deposition (UPD) on the prepared films. Integrated Pb UPD charge values of ca. 1600 to 4000 µC/cm2 for the prepared Cu-Au films have been calculated, suggesting a 5 to 14-fold increase of the active surface area compared to flat surfaces of polycrystalline Cu or Au. These results show that metal electrodeposition in DES allows the preparation of high extended surface area bimetallic nanomaterials in an environmentally friendly route.


We gratefully acknowledge the Villum Foundation for financial support through a Villum Young Investigator Grant (project number: 19142).  This work was also supported by the Danish foundation through the DFF-Research Project1 (Thematic Research, green transition) grant with number: 0217-00213A; and the DFF-grant Project 1 with number 9041-00224B. We acknowledge support from the Danish National Research Foundation Center for High Entropy Alloy Catalysis (CHEAC, DNRF-149). We also acknowledge Prof. Elvira Gómez from University of Barcelona who provided valuable experimental discussions.

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