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Pulsed galvanostatic and potentiostatic electrodeposition of Cu and Cu2O nanolayers from alkaline Cu(II)-citrate solutions
Uppsala University, Disciplinary Domain of Science and Technology, Chemistry, Department of Materials Chemistry.
Uppsala University, Disciplinary Domain of Science and Technology, Chemistry, Department of Materials Chemistry.
2008 (English)In: Journal of the Electrochemical Society, ISSN 0013-4651, Vol. 155, no 2, D115-D122 p.Article in journal (Refereed) Published
Abstract [en]

Nanolayers of Cu and Cu2O with a wide range of layer thicknesses have been produced using pulsed galvanostatic and potentiostatic electrodeposition from alkaline Cu(II)-citrate solutions. The thicknesses of the individual Cu and Cu2O layers can be independently controlled and the composition of the multilayered materials, which also were studied using electrochemical quartz crystal microbalance, X-ray diffraction, and scanning electron microscopy, can be varied from pure Cu to pure Cu2O by varying the current density or the deposition potential. It is shown that some of the deposited Cu2O is reduced during the subsequent copper deposition step and that the influence of this effect depends on the Cu (II) concentration, the Cu2O microstructure, and the deposition mode. Additional Cu2O deposition is demonstrated to take place after the copper deposition step due to comproportionation and precipitation of Cu2O. This effect facilitates electrodeposition of Cu2O on Cu. Deposition of Cu on the Cu2O layer formed by comproportionation and precipitation was likewise found to be more straightforward than on electrodeposited Cu2O. Well-defined nanolayered Cu/Cu2O materials are generally best manufactured using pulsed galvanostatic techniques because a much larger fraction of the Cu2O was found to be reduced during the subsequent Cu deposition pulse in pulsed potentiostatic depositions.

Place, publisher, year, edition, pages
2008. Vol. 155, no 2, D115-D122 p.
National Category
Chemical Sciences
URN: urn:nbn:se:uu:diva-96154DOI: 10.1149/1.2806793ISI: 000251906800038OAI: oai:DiVA.org:uu-96154DiVA: diva2:170632
Available from: 2007-09-07 Created: 2007-09-07 Last updated: 2013-04-04Bibliographically approved
In thesis
1. Electrochemical Deposition of Nanostructured Metal/Metal-Oxide Coatings
Open this publication in new window or tab >>Electrochemical Deposition of Nanostructured Metal/Metal-Oxide Coatings
2007 (English)Doctoral thesis, comprehensive summary (Other academic)
Abstract [en]

Electrochemical deposition finds applications in the electronics- and protective coating industries. The technique is a versatile tool for the synthesis of alloys and thin films. Knowledge of the fundamental aspects of the electrode processes enables the design of nanostructured materials. In this thesis, electrodeposition processes in solutions containing metal ion complexes were studied and new methods for the preparation of metal/metal-oxide coatings were developed and evaluated.

Metal/metal oxide coatings were electrodeposited from aqueous solutions containing metal complexes of hydroxycarboxylic acids under reducing conditions. The mass changes of the working electrode were monitored in-situ with the electrochemical quartz crystal microbalance (EQCM) technique and ellipsometry was used to detect the formation of Cu2O. The coatings were further characterized with XRD, XPS, SEM, TEM, and Raman spectroscopy. Electrochemical methods, including reduction of Sb/Sb2O3 in an organic electrolyte, were also used to study the properties of the deposited materials.

Nanostructured coatings of Cu/Cu2O were obtained during spontaneous potential or current oscillations in alkaline Cu(II)-citrate solutions. The oscillations were due to local pH variations induced by a subsequent chemical step and comproportionation between Cu and Cu2+. Well-defined layers of Cu and Cu2O could be prepared by a galvanostatic pulsing technique, allowing independently controlled thickness of several hundred nanometers. Coatings, containing Sb and co-deposited, nanograins of Sb2O3, with a thickness of up to 200 nm were prepared from poorly buffered Sb(III)-tartrate solutions. Galvanostatic cycling showed that the latter material could be reversibly charged and discharged in a Li-ion battery for more than 50 cycles with a capacity of 660 mAh/g.

The results show that precipitations of metal oxides can occur due to local pH increases during electrochemical deposition from metal complexes with ligands containing hydroxyl groups. The ability to deposit metal oxides using cathodic deposition relies on a sufficiently slow reduction of the oxide.

Place, publisher, year, edition, pages
Uppsala: Acta Universitatis Upsaliensis, 2007. 54 p.
Digital Comprehensive Summaries of Uppsala Dissertations from the Faculty of Science and Technology, ISSN 1651-6214 ; 336
Inorganic chemistry, electrochemical deposition, local pH, Cu2O, Sb2O3, complex, EQCM, reduction, Oorganisk kemi
urn:nbn:se:uu:diva-8186 (URN)978-91-554-6956-6 (ISBN)
Public defence
2007-09-28, Häggsalen, Ångströmlaboratoriet, Lägerhyddsvägen 1, Uppsala, 14:00
Available from: 2007-09-07 Created: 2007-09-07 Last updated: 2011-03-25Bibliographically approved

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Nyholm, Leif
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