Data from: Electrodeposition of iron from 1-ethyl-3-methylimmidazolium trifluoromethanesulphonate and reverse microemulsions of Triton X-100

Tabassum, Nazifa1 ; Saha, Shimul2; Islam, Md. Mominul1 ; Susan, Md. Abu Bin Hasan1

Published May 08, 2024 on Dryad. https://doi.org/10.5061/dryad.47d7wm3k6

Abstract

Electrodeposition of iron (Fe) was investigated in three different media: namely, a hydrophilic ionic liquid (IL), 1-ethyl-3-methylimmidazolium trifluoromethanesulphonate, conventional reverse microemulsion (RME)/reverse micellar solution, and IL based reverse microemulsion of a non-ionic surfactant, Triton X-100 with a view to achieving control over size, shape, and morphology of the electrodeposited iron. Electrochemical behavior of Fe²⁺was studied using cyclic voltammetric technique with a copper electrode as the working electrode. Electrochemical reduction of Fe²⁺ in all the studied media was found to be an electrochemically irreversible, diffusion-controlled process. Successful potentiostatic electrodeposition of metallic iron was performed in all the studied media on copper substrate using bulk electrolysis method. The obtained iron electrodeposits were characterized using a scanning electron microscope (SEM) and an x-ray diffractometer (XRD). The controlled diffusion of Fe²⁺ towards electrode surfacein all the media resulted in the formation of nanoparticles of iron, but compact layers of granular nanoparticles could be achieved from both the conventional and IL based RME systems. The IL based microemulsions synergistically combined the advantageous features of both the IL and RME and showed the prospect of tuning the size, shape, and morphology of the electrodeposited iron.

README: Data from: Electrodeposition of iron from 1-ethyl-3-methylimmidazolium trifluoromethanesulphonate and reverse microemulsions of Triton X-100

The electrochemical measurements and electrodeposition were carried out with a computer-controlled electrochemical analyzer (Model: CHI 660E and CHI 760E, CH Instruments, Inc., USA) using a conventional single-compartment three-electrode cell. Prior to each measurement, the solution was purged with nitrogen gas to maintain an inert atmosphere during the course of the measurement. A homemade copper disc electrode (d = 1 mm) was used as the working electrode during cyclic voltammetric measurements. The electrode was mechanically polished using 0.05 m alumina paste (Buehler, country) to obtain a uniform surface and then rinsed thoroughly with distilled water and dried. The dried electrode was then introduced into the cell filled with the test solution. A platinum (Pt) wire was used as the counter electrode. A Ag/AgCl was used as the reference electrode in the conventional RMEs, while a Ag wire was used in the IL and IL-RME systems. The Ag/AgCl reference electrode used in the conventional RMEs was found to be fairly stable during the course of the experiments which was judged by comparing the cyclic voltammograms performed at different time intervals. Metallic iron deposits were obtained on a copper substrate (d = 6 mm) with bulk electrolysis by applying constant potential using the same three-electrode single-compartment cell used for cyclic voltammetric measurements.

The crystalline structure of the deposits was investigated by an x-ray diffractometer (Rigaku Smartlab SE, Japan).

Description of the data and file structure

Data from cyclic volttamograms (current, potential at different scan rates) were used for the plots for Fig. 1, 1 (a), (b),5 (a), (b), 6(a), (b), 7(a), (b) and S1. Intensity at different diffraction angles were used from XRD pattern for Fig. 4.

Fig. 1 Cyclic voltammograms of 10 mM FeSO4 in [emim][TfO] at different scan rates on a copper electrode at 30 oC. The solid black line shows the cyclic voltammogram in neat [emim][TfO].

Fig. 2 (a) Variation of cathodic peak potentials with the logarithms of scan rates and (b) Variation of cathodic peak currents with the squire root of scan rates for the cyclic voltammogram of 10 mM FeSO4 in [emim][TfO] on a copper electrode at 30 oC.

Fig. 4 XRD pattern of iron deposit obtained by potentiostatic electrolysis at -0.6 V for 1 h on a copper substrate in [emim][TfO] containing 10 mM FeSO4.

Fig. 5 Cyclic voltammograms of (a) 3 mM FeSO4 in RME of TX-100, (b) 20 mM FeSO4 in IL based RME of TX-100 at different scan rates on a copper electrode at 30 oC.

Fig. 6 Variation of cathodic peak potentials with the logarithms of scan rates for the cyclic voltammograms of (a) 3 mM FeSO4 in conventional RME of TX-100 and (b) 20 mM FeSO4 in IL-RME of TX-100 on a copper electrode at 30 oC.

Fig. 7 Variation of cathodic peak currents with the squire root of scan rates for the cyclic voltammograms of (a) 3 mM FeSO4 in conventional RME of TX-100 and (b) 20 mM FeSO4 in IL-RME of TX-100 on a copper electrode at 30 oC.

Figure S1: Cyclic voltammograms of 80 mM FeSO4 in aqueous medium containing Na2SO4 as supporting electrolyte at different scan rates on a copper electrode at 30 oC. The solid black line shows the cyclic voltammogram in the absence of FeSO4.

Sharing/Access information

All data are accessible through the shared datasets

Code/Software

SigmaPlot 11 software will be required to access the data. Extension of fil i .JNB. The Supplementary information is available as a word file with the dataset for Fig. S1 made available. CSV files will allow free acees and therefore these files are also added.