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Publication details

Document type
Journal articles

Document subtype
Full paper

Title
Real-time in situ dynamic sub-surface imaging of multi-component electrodeposited films using event mode neutron reflectivity

Participants in the publication
A. Robert Hillman (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 - Centro de Química e Bioquímica 
Emma J. R. Palin (Author)
Rachel M. Sapstead (Author)
Emma L. Smith (Author)
Nina-Juliane Steinke (Author)
Karl S. Ryder (Author)
Andrew D. Ballantyne (Author)

Scope
International

Refereeing
Yes

Summary
Exquisite control of the electrodeposition of metal films and coatings is critical to a number of high technology and manufacturing industries, delivering functionality as diverse as anti-corrosion and anti-wear coatings, electronic device interconnects and energy storage. The frequent involvement of more than one metal motivates the capability to control, maintain and monitor spatial disposition of the component metals, whether as multilayers, alloys or composites. Here we investigate the deposition, evolution and dissolution of single and two-component metal layers involving Ag, Cu, and Sn on Au substrates immersed in the deep eutectic solvent (DES) Ethaline. During galvanostatically controlled stripping of the metals from two-component systems the potential signature in simultaneous thickness electrochemical potential (STEP) measurements provides identification of the dissolving metal; coulometric assay of deposition efficiency is an additional outcome. When combined with quartz crystal microbalance (QCM) frequency responses, the mass change : charge ratio provides oxidation state data; this is significant for Cu in the high chloride environment provided by Ethaline. The spatial distribution (solvent penetration and external roughness) of multiple components in bilayer systems is provided by specular neutron reflectivity (NR). Significantly, the use of the recently established event mode capability shortens the observational timescale of the NR measurements by an order of magnitude, permitting dynamic in situ observations on practically useful timescales. Ag,Cu bilayers of both spatial configurations give identical STEP signatures indicating that, despite the extremely low layer porosity, thermodynamic constraints (rather than spatial accessibility) dictate reactivity; thus, surprisingly, Cu dissolves first in both instances. Sn penetrates the Au electrode on the timescale of deposition; this can be prevented by interposing a layer of either Ag or Cu.

Date of Submisson/Request
2018-04-24
Date of Acceptance
2018-04-25
Date of Publication
2018-00-00

Institution
FACULDADE DE CIÊNCIAS DA UNIVERSIDADE DE LISBOA

Where published
Faraday Discussions

Publication Identifiers
ISSN - 1359-6640

Publisher
Royal Society of Chemistry (RSC)

Volume
210

Starting page
429
Last page
449

Document Identifiers
URL - http://dx.doi.org/10.1039/c8fd00084k
DOI - https://doi.org/10.1039/c8fd00084k

Rankings
SCOPUS Q1 (2017) - 1.458 - Physical and Theoretical Chemistry
SCIMAGO Q1 (2017) - 1.458 - Physical and Theoretical Chemistry
SCOPUS Q1 (2016) - 1.524 - Physical and Theoretical Chemistry

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APA
A. Robert Hillman, Robert Barker, Robert M. Dalgliesh, Virginia C. Ferreira, Emma J. R. Palin, Rachel M. Sapstead, Emma L. Smith, Nina-Juliane Steinke, Karl S. Ryder, Andrew D. Ballantyne, (2018). Real-time in situ dynamic sub-surface imaging of multi-component electrodeposited films using event mode neutron reflectivity. Faraday Discussions, 210, 429-449. ISSN 1359-6640. eISSN . http://dx.doi.org/10.1039/c8fd00084k

IEEE
A. Robert Hillman, Robert Barker, Robert M. Dalgliesh, Virginia C. Ferreira, Emma J. R. Palin, Rachel M. Sapstead, Emma L. Smith, Nina-Juliane Steinke, Karl S. Ryder, Andrew D. Ballantyne, "Real-time in situ dynamic sub-surface imaging of multi-component electrodeposited films using event mode neutron reflectivity" in Faraday Discussions, vol. 210, pp. 429-449, 2018. 10.1039/c8fd00084k

BIBTEX
@article{37311, author = {A. Robert Hillman and Robert Barker and Robert M. Dalgliesh and Virginia C. Ferreira and Emma J. R. Palin and Rachel M. Sapstead and Emma L. Smith and Nina-Juliane Steinke and Karl S. Ryder and Andrew D. Ballantyne}, title = {Real-time in situ dynamic sub-surface imaging of multi-component electrodeposited films using event mode neutron reflectivity}, journal = {Faraday Discussions}, year = 2018, pages = {429-449}, volume = 210 }