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Stainless steel substrate pretreatment effects on copper nucleation and stripping during copper electrowinning

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Abstract

The effects of surface pretreatment of 304 stainless steel (SS) substrates on copper film formation, adhesion, and purity obtained by galvanostatic electrodeposition at a current density of – 30 mA cm−2 are presented. The polished substrate produced more copper nuclei, resulting in an increase of the adhesion as compared to chemically oxidized SS substrate. The adhesion of the copper deposits was characterized by a Nano-scratch tester (NST). The nucleation behavior is associated with the flatband potential of the SS surface, which was derived from capacitance measurements. The grain size of copper deposits was characterized by field emission scanning electron microscopy (FESEM). Copper grains were smaller on the polished SS with a size of less than 1 µm after 5 min of electrodeposition. High-purity copper deposits with < 1 ppm S (detection limit) were obtained on the oxidized SS substrate compared to 2.5 ppm for the polished SS substrate. Atomic force microscopy (AFM) measurements showed that the copper deposits were 25% less rough on the polished SS as compared to the oxidized SS. The results indicate that the obtained purity of the copper deposit relates to the grain size of the deposit, rather than the initial surface roughness. In the context of industrial electrowinning, high adherence to the polished substrate could increase the operation time of the copper cathode stripping. Hence for electrowinning from copper sulfate electrolytes, oxidizing the SS surface prior to deposition could lead to higher purity along with enhanced stripping.

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The datasets generated during and/or analyzed during the current study are available from the corresponding author on reasonable request.

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The custom made software used in the study is available from the corresponding author on reasonable request.

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Acknowledgements

This research was financially supported by the Flemish Agency for Innovation and Entrepreneurship (Vlaio) via a Baekeland PhD fellowship to Florian Verbruggen (HBC.2017.0224) and by the Research & Development Umicore Group. EF is supported by the Fonds voor Wetenschappelijk Onderzoek - Vlaanderen (FWO) PROJECT G020616N. KR and AP are supported by a Ghent University Bijzonder Onderzoeksfonds GOA grant (BOF19/GOA/026). LB is supported by the Fonds voor Wetenschappelijk Onderzoek - Vlaanderen (FWO) PROJECT 3G0I1818W. The authors thank Umicore for the permission to publish the results. We gratefully acknowledge Louis Van der Meeren for performing the AFM measurements.

Funding

This research was financially supported by the Flemish Agency for Innovation and Entrepreneurship (Vlaio) via a Baekeland PhD fellowship to Florian Verbruggen (HBC.2017.0224) and by the Research & Development Umicore Group. EF is supported by the Fonds voor Wetenschappelijk Onderzoek - Vlaanderen (FWO) PROJECT G020616N. KR and AP are supported by a Ghent University Bijzonder Onderzoeksfonds GOA grant (BOF19/GOA/026). LB is supported by the Fonds voor Wetenschappelijk Onderzoek - Vlaanderen (FWO) PROJECT 3G0I1818W.

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  1. Erika Fiset

    Present address: BOSAQ, Technologiepark 82 POB 7, 9052, Zwijnaarde, Belgium

Authors and Affiliations

  1. Center for Microbial Ecology and Technology (CMET), Ghent University, Coupure Links 653, 9000, Ghent, Belgium

    Florian Verbruggen, Erika Fiset, Luiza Bonin, Antonin Prévoteau, Tom Hennebel & Korneel Rabaey

  2. CAPTURE, Ghent, Belgium

    Florian Verbruggen, Erika Fiset, Luiza Bonin, Antonin Prévoteau, Tom Hennebel & Korneel Rabaey

  3. Umicore, Group Research & Development, Competence Area Recycling and Extraction Technologies, Watertorenstraat 33, 2250, Olen, Belgium

    Tom Hennebel

  4. Materials Research Center, Missouri S&T, Rolla, MO, 65401, USA

    Michael S. Moats

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FV: conceptualization, methodology, validation, formal analysis, investigation, writing—original draft, and visualization. EF: methodology, validation, writing, review & editing. LB: investigation, methodology, validation, writing, review & editing. AP: methodology, validation, writing, review & editing. MSM: supervision, resources, review & editing, and conceptualization. TH: supervision, project administration, resources, and conceptualization. KR: supervision, project administration, resources, visualization, and review. 

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Verbruggen, F., Fiset, E., Bonin, L. et al. Stainless steel substrate pretreatment effects on copper nucleation and stripping during copper electrowinning. J Appl Electrochem 51, 219–233 (2021). https://doi.org/10.1007/s10800-020-01485-2

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