Abstract: The electrochemical reduction of CO2 represents an attractive alternative to both, satisfy the increasing energy demand, and to help closing the carbon cycle. However, the energy required for CO2 activation and the subsequent multiple number of proton-coupled electron transfer steps involved, makes this process very challenging. Besides, catalytic material limitations are hampering the application of this technology in the short term. Consequently, in this work we synthesise, characterise and preliminarily evaluate bimetallic Cu-based hollow fibre electrodes with a compact three-dimensional geometry to overcome mass transfer limitations and to enhance the electrochemical conversion of CO2. The Cu hollow fibres are functionalised with Au in an attempt to tune the binding energy of the CO* intermediate, which appears to be key in the reduction of CO2. The Cu fibres are also functionalised with Ni, aiming to decrease the reaction overpotential, resulting in beneficial energy efficiency. The so prepared Cu-based porous hollow fibre electrodes are obtained by spinning and electrodeposition procedures. The materials are then characterised by scanning electron microscopy, energy dispersive X-ray spectroscopy, Xray diffraction analyses and cyclic voltammetry tests. Finally, preliminary results of CO2 electroreduction in a divided three-electrode cell are reported. The results show the potential of highly active, bimetallic hollow fibre-based electrocatalysts for enhanced conversion of CO2 into value-added products, and deposition of particles should be performed with acre, not to effect pore characteristics and thus mass transfer properties.

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