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

Ballantyne, A. D., Barker, R., Dalgliesh, R. M., Ferreira, V. C., Hillman, A. R., Palin, E. J. R., Sapstead, R., Smith, E. L., Steinke, N.-J. and Ryder, K. S. (2018) Electrochemical deposition of silver and copper from a deep eutectic solvent studied using time-resolved neutron reflectivity. Journal of Electroanalytical Chemistry. 819, 511 - 523. 1572-6657.

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Item Type:	Article
Abstract:	Here, we describe new developments in the study of electrodeposition processes with time-resolved dynamicneutron reﬂectivity (NR) methods to achieve insights into the diﬀerences between growth of metal ﬁlms using arange of electrochemical control functions. We show that the temporal resolution has increased from 1 to 2 h perdata set (in our previous studies) to approximately 8 min. We have studied the electrochemical deposition ofcopper and silver as thin-ﬁlm metals onto a gold electrode substrate from a deep eutectic solvent using po-tentiodynamic (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 growingmetal 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), proﬁlesof 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 datashow that the di ﬀerent electrochemical growth methodologies exhibit diﬀerent trends in thickness, roughnessand 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, showsa strong dependency on growth method with PS methods producing smoothest ﬁlms. These conclusions areconﬁrmed 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 inorder to process the large numbers of data sets produced. Gratifyingly, the diﬀerent methodologies and startingconditions yield a very consistent picture of metal ﬁlm growth.
Uncontrolled Keywords:	Neutron reflectivity, electrodeposition, deep eutectic solvents, copper, silver, thin-film, cyclic voltammetry, atomic force microscopy
Subjects:	T Technology > TP Chemical technology > TP250 Industrial electrochemistry
Creators:	Ballantyne, Andrew D, Barker, Robert, Dalgliesh, Robert M, Ferreira, Virginia C, Hillman, A Robert, Palin, Emma J R, Sapstead, Rachel, Smith, Emma L, Steinke, Nina-Juliane and Ryder, Karl S
Publisher:	Elsevier
Faculties, Divisions and Institutes:	Research Institutes > Institute for Creative Leather Technologies
Date:	15 June 2018
Date Type:	Publication
Page Range:	511 - 523
Journal or Publication Title:	Journal of Electroanalytical Chemistry
Volume:	819
Language:	English
DOI:	https://doi.org/10.1016/j.jelechem.2018.01.032
ISSN:	1572-6657
Status:	Published / Disseminated
Refereed:	Yes
URI:	http://nectar.northampton.ac.uk/id/eprint/10463

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