In situ scanning tunneling microscopy (STM), atomic force microscopy (AFM) and quartz crystal microbalance (EQCM) studies of the electrochemical deposition of tantalum in two different ionic liquids with the 1-butyl-1-methylpyrrolidinium cation

The electrochemical reduction of 0.1M TaF5 in two hydrophobic ionic liquids (1-butyl-1-methylpyrrolidinium tris(pentafluoroethyl) trifluorophosphate ([Py1,4]FAP) and 1-butyl-1-methylpyrrolidinium bis(trifluoromethylsulfonyl) amide ([Py1,4]TFSA) is probed using three in situ techniques: scanning tunn...

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Bibliographic Details
Published in:Electrochimica acta 2016-04, Vol.197, p.374-387
Main Authors: Carstens, Timo, Ispas, Adriana, Borisenko, Natalia, Atkin, Rob, Bund, Andreas, Endres, Frank
Format: Article
Language:English
Subjects:
AFM
Atomic force microscopy
Deposition
Electrodeposition
Ionic liquid
Ionic liquids
Liquids
Microbalances
Quartz crystals
Scanning tunneling microscopy
STM
Tantalum
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Summary:The electrochemical reduction of 0.1M TaF5 in two hydrophobic ionic liquids (1-butyl-1-methylpyrrolidinium tris(pentafluoroethyl) trifluorophosphate ([Py1,4]FAP) and 1-butyl-1-methylpyrrolidinium bis(trifluoromethylsulfonyl) amide ([Py1,4]TFSA) is probed using three in situ techniques: scanning tunneling microscopy (STM), atomic force microscopy (AFM), and electrochemical quartz crystal microbalance (EQCM). These techniques reveal that under similar conditions TaF5 is more easily reduced in the liquids with [TFSA]− than [FAP]−anions. Increasing the temperature reduced the viscosity and density of the ionic liquids which facilitates TaF5 electroreduction, in particular, in [Py1,4]TFSA. A herringbone reconstruction of the Au electrode was observed by STM for both ionic liquids with and without TaF5. Ta deposition was proved by STM and EQCM in [Py1,4]TFSA. Cracked layers, with ionic liquid trapped inside, were obtained by direct plating from the [TFSA]− ionic liquid. No Ta containing deposits could be obtained in the liquid with the [FAP]− anion.
ISSN:0013-4686
1873-3859
DOI:10.1016/j.electacta.2015.07.178