BIBLIOS

Document type
Journal articles

Document subtype
Full paper

Title
Electrochemical deposition of silver and copper from a deep eutectic solvent studied using time-resolved neutron reflectivity

Participants in the publication
Andrew D. Ballantyne (Author)
Robert Barker (Author)
Robert M. Dalgliesh (Author)
Virginia C. Ferreira (Author)
FACULDADE DE CIÊNCIAS DA UNIVERSIDADE DE LISBOA
Dep. Química e Bioquímica
Dep. Química e Bioquímica
CQB
A. Robert Hillman (Author)
Emma J.R. Palin (Author)
Rachel Sapstead (Author)
Emma L. Smith (Author)
Nina-Juliane Steinke (Author)
Karl S. Ryder (Author)

Summary
Here, we describe new developments in the study of electrodeposition processes with time-resolved dynamic neutron reflectivity (NR) methods to achieve insights into the differences between growth of metal films using a range of electrochemical control functions. We show that the temporal resolution has increased from 1 to 2 h per data set (in our previous studies) to approximately 8 min. We have studied the electrochemical deposition of copper and silver as thin-film metals onto a gold electrode substrate from a deep eutectic solvent using potentiodynamic (PD), potentiostatic (PS) and galvanostatic (GS) electrochemical control functions. In particular,we have utilised novel developments in neutron reflectivity methods to acquire real-time data for the growing metal films.Event mode capture of neutron scattering events, as a function of momentum transfer vector, Q, during electrochemical growth has enabled time-resolved measurement of the neutron reflectivity, R(Q), profiles of the growing metal films. Subsequent fitting and iterative optimisation of the R(Q,t) data reveals the thickness,roughness and relative density (spatially resolved solvent content) of the metal film during growth. These data show that the different electrochemical growth methodologies exhibit different trends in thickness, roughness and solvation. Silver films show an increasing roughness trend with time but these trends are largely in-dependent of growth method. In contrast, the roughness of copper films, grown under similar conditions, shows a strong dependency on growth method with PS methods producing smoothest films. These conclusions are confirmed by ex-situ AFM measurements. The fitted NR data show that the Cu and Ag films contain between 5and 10% volume fraction solvent. Furthermore, we have explored different NR data fitting methodologies in order to process the large numbers of data sets produced. Gratifyingly, the different methodologies and starting conditions yield a very consistent picture of metal film growth.


Institution
FACULDADE DE CIÊNCIAS DA UNIVERSIDADE DE LISBOA

Where published
Journal of Electroanalytical Chemistry

Publication Identifiers
ISSN - 1572-6657

Publisher
Elsevier BV



Document Identifiers
URL - http://dx.doi.org/10.1016/j.jelechem.2018.01.032
DOI - https://doi.org/10.1016/j.jelechem.2018.01.032

Rankings
SCIMAGO Q1 (2018) - 0.727 - Chemical Engineering (miscellaneous)
SCOPUS Q1 (2017) - 0.765 - General Chemical Engineering

Keywords
Atomic force microscopy Cyclic voltammetry Deep eutectic solvents Electrodeposition Event mode Neutron reflectivity Copper Silver Thin-film

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