ISSN 0321-4095, Voprosy Khimii i Khimicheskoi Tekhnologii, 2022, No. 2, pp.

3-8

UDC 544.65

Initial stages of electrocrystallization of nickel, iron and nickel-iron

alloy on a glassy carbon electrode in an electrolyte based on a eutectic
mixture of choline chloride and ethylene glycol
F.I. Danilov, D.A. Bogdanov, V.S. Protsenko
Ukrainian State University of Chemical Technology, Dnipro, Ukraine
The kinetics and mechanism of the initial stages of electrocrystallization of nickel, iron and nickel-iron alloy were characterized for
the process of electrolytic deposition from a solution based on deep eutectic solvent ethaline (liquid mixture containing choline
chloride and ethylene glycol at a molar ratio of 1:2, respectively). The theoretical model developed by Scharifker and Hills was
used to interpret the obtained experimental data. It was shown that the electrodeposition of nickel and iron obeys the patterns of
three-dimensional instantaneous and progressive nucleation, respectively. It was concluded that the formation of iron nuclei
occurs at a significantly lower rate than in the case of nickel. The kinetics of the initial stages of Ni–Fe alloy deposition obeys the
mechanism of instantaneous nucleation. Thus, in the case of electrolytic deposition from ethaline-based solutions on a glassy
carbon electrode, nickel imposes on iron not only its own region of electrode potentials where alloy deposition occurs, but also
the type of mechanism of nucleation in the course of codeposition.

Keywords: electrochemical crystallization, nickel, iron, alloy, deep eutectic solvent.

DOI: 10.32434/0321-4095-2022-141-2-3-8

contradictory [7,10–12]. In particular,

Introduction electrocrystallization of nickel from an electrolyte
based on reline (a DES, which is a eutectic mixture
Studying the electrochemical deposition of metal of choline chloride and urea) on a copper
coatings from electrolytes based on the so-called microelectrode obeys the patterns of three-
deep eutectic solvents (DESs) is currently one of dimensional instantaneous nucleation, the nature
the key trend in modern electrochemical science of which does not change with the introduction of
[1,2]. Among the wide range of various metals nicotinic acid [10]. However, in the study of the
and alloys that can be electrodeposited from this initial stages of Ni electrocrystallization from the
type of room-temperature ionic liquids, nickel, same electrolyte on a glassy carbon electrode and
iron and nickel-iron alloy occupy a special place controlled water content in solution [11], it was
due to a unique combination of corrosion, found that both instantaneous and progressive
protective, mechanical, electrocatalytic, magnetic nucleation mechanisms can be observed,
and other properties of coatings [3–7]. Earlier [8], depending on the selected potential applied to
we considered the kinetics of codeposition of the electrode. Patterns of electrochemical
nickel and iron from the electrolyte based on a nucleation of nickel in ethaline-based solutions
widespread representative of DESs, the so-called are not described in the literature.
ethaline, which is a eutectic mixture of choline As for the deposition of iron, it was shown that
chloride and ethylene glycol. It was shown that the mechanism of progressive nucleation is
the process of electrolytic deposition of Ni–Fe realized in the ethaline-based solution on a glassy
alloy from this electrolyte is accompanied by carbon electrode [7,12]. However, the process is
acceleration of the discharge of iron (II) ions. A sensitive to the chemical composition of the
mechanism based on the ideas previously electrolyte (for example, in a solution with a
reported by Zech et al. [9] was proposed to reduced concentration of chloride ions, the
explain this effect. However, the patterns of the process is not described by either the mechanism
initial crystallization stages, the kinetics of which of progressive nucleation or instantaneous one).
are extremely sensitive to the nature of the Since an electrolyte containing an ascorbic acid
electrolyte used, was left out of consideration. additive was used in our study [8] to prevent the
Currently available data on the oxidation of iron(II) ions by atmospheric oxygen, it
electrocrystallization stages of deposition of remains unclear whether the conclusions about
nickel and iron from DESs are rather limited and the electrocrystallization mechanism reported in
 F.I. Danilov, D.A. Bogdanov, V.S. Protsenko, 2022

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Voprosy Khimii i Khimicheskoi Tekhnologii, 2022, no. 2, pp. 3-8

–3
works [7,12] can be extended a priori to the immersed in a solution of 2.5 mmol dm
–3
deposition process of iron from the electrolyte K3[Fe(CN)6]+2.5 mmol dm K3[Fe(CN)6] in
used in study [8]. Patterns of electrochemical ethaline, which was at the same temperature as
nucleation during deposition of Ni–Fe alloy from working electrode. The electrical contact of the
DES-based electrolytes are not described in the solution in which the reference electrode was
literature known to us. located and the solution in which the working and
In view of the above, the aim of this work was to auxiliary electrodes were immersed was provided
establish the patterns of the initial stages of by the Luggin capillary.
electrochemical crystallization in the course of Current transients in the study of
nickel, iron and nickel-iron alloy deposition from electrocrystallization were recorded in
an electrolyte based on eutectic mixture ethaline potentiostatic mode using the
containing the additive of ascorbic acid. Potentiostat/Galvanostat/ZRAReference 3000
(Gamry, USA).

Experimental
Electrolytes containing 0.5 M NiCl2 (for deposition
Results and discussion
of individual nickel), 0.2 M FeCl2H2O (for The experimentally registered current density
deposition of individual iron) or 0.5 M transients for the initial stages of
NiCl2+0.2 M FeCl2H2O (for deposition of Ni–Fe electrocrystallization of nickel, iron, and Ni–Fe
alloy) in ethaline were used for coatings alloy for different electrode potentials are shown
preparation. All electrolytes also contained an in Fig. 1. All the obtained transients have a
–3
additive of ascorbic acid (2 g dm ), which is classical appearance: the initial increase in
introduced to prevent spontaneous oxidation of current after the imposition of the cathode
iron(II) ions caused by the interaction with electrode potential, reaching a certain maximum
atmospheric oxygen. The method of preparation value of current density (imax), which corresponds
of the electrolytes was described in detail in our to a certain point in time (t max), and a further
previous publication [8]. It should be observed decrease in current density. An increase in the
that, as found out earlier [8], the presence of current density at tmax<0 is due to an increase in
water impurities in the electrolyte based on a DES the surface concentration of the nuclei of the
can affect the kinetics and mechanism of metal phase formed on the electrode. A decrease
electrochemical processes. That is why we used in the current density at tmax>0 is determined by a
anhydrous nickel chloride salt and iron chloride decrease in the concentration of discharged metal
monohydrate, rather than the more common and ions due to diffusion limitations of their transport.
available suitable crystal hydrates with higher In all cases, other things being equal, an increase
water content. According to our calculations, the in the cathodic polarization leads to an increase in
introduction of water of crystallization via the the maximum current density (imax) and a
addition of the specified amount of iron(II) decrease in the corresponding time (tmax). It
chloride monohydrate increases the water should be noted that the electrocrystallization of
content by 0.4 wt.%. Due to the hygroscopicity of individual iron occurs at electrode potentials
the components of the solution, the electrolytes significantly more negative than in the case of
contained a certain amount of water, the total individual nickel, which is fully consistent with the
content of which did not exceed 1 wt.% results of previous voltammetric studies [8].
(determined by the Fisher method). Electrodeposition of the Ni–Fe alloy occurs at
A glassy carbon working electrode ( 3 mm) was potentials close to the value inherent in nickel
used to record current transients, the surface of [8,13].
the electrode being polished and washed in To quantify the obtained current transients, we
hydrochloric acid solution before each used the known kinetic model developed by
experiment, then with distilled water and dried in Scharifker and Hills [14]. This model describes two
an air stream. The experiments were performed different mechanisms of formation of a
0
in a common thermostated (60 C) three- monolayer of metal nuclei during
electrode cell. The auxiliary electrode was either a electrodeposition on a foreign substrate:
nickel plate (in the study of electrocrystallization (i) instantaneous nucleation, when almost all
of nickel and nickel-iron alloy) or a steel plate (in nuclei are formed immediately after switching on
the study of electrocrystallization of iron). The the cathode current (this means a high rate of
reference electrode was a platinum wire nucleation as compared with the rate of their

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 Voprosy Khimii i Khimicheskoi Tekhnologii, 2022, no. 2, pp. 3-8

subsequent growth); and (ii) progressive Let us note that these two mechanisms are both
nucleation, when the number of nuclei gradually ideal cases, and in practice a certain combination
increases over time during electrodeposition (this of these two extreme cases can be realized, when
means a relatively low rate of nucleation). one of them prevails.
i, mA
In order to determine which nucleation
-2.0 mechanism is valid for this particular case, it is
5
customary to use the following kinetic equations
Ni in dimensionless form [14]:
-1.5
4
2
 i  1.9542    t   , (1)
2

3
   1  exp 1.2564  
-1.0  imax  t tmax    tmax  
2
1 2
 i  1.2254    t    . (2)
2 2
-0.5
   1  exp  2.3367 
 t  
 imax  t tmax 
 
  max   
0.0
0 2 4 6 8 10 12 14 16
Equations (1) and (2) describe the kinetics of
t, s
instantaneous and progressive nucleation,
a respectively. The graph plotted in dimensionless
2
coordinates (i/imax) vs. (t/tmax) according to Eqs.
i, mA
-2.0
(1)–(2) yields two lines (Fig. 2), the appearance
and location of which do not depend on the
electrode potential. These two curves allow
-1.5 Fe discriminating between two nucleation
2
9
mechanism: if the dependence (i/imax) vs. (t/tmax)
8
plotted on the basis of experimental data
-1.0 7
6
approaches that reflected by Eq. (1), then a
conclusion is made about the instantaneous
-0.5 mechanism of nucleation. If the obtained
experimental data are more accurately reflected
by the curve corresponding to Eq. (2), it indicates
0.0
0 2 4 6 8 10 12 14 16 a progressive mechanism of nucleation.
t, s Analysis of the obtained data shows that the
electrocrystallization of individual nickel obeys
b the patterns of instantaneous nucleation
i, mA (Fig. 2,a), which coincides with the mechanism
-2.0 reported for the nickel plating electrolyte based
on reline [10]. Interestingly, the value of the
-1.5 Ni-Fe deposition potential (in the studied range from –
0.89 V to –1.01 V) has little effect on the
13 appearance and location of these test curves in
2
-1.0
12 dimensionless coordinates (i/imax) vs. (t/tmax).
11 The electrocrystallization of individual iron on a
10 glassy carbon electrode is fundamentally
-0.5
different. Although the scatter of the points of
2
the corresponding curves (i/imax) vs. (t/tmax) when
0.0 varying the electrode potential is significantly
0 2 4 6 8 10 12 14 16
larger (Fig. 2,b), the nature of the dependences
t, s
allows us to draw a clear conclusion about the
c mechanism of progressive nucleation. This finding
Fig. 1. Current transients for the initial stages of electrocrystallization coincides with the conclusion made earlier in
for deposition of Ni (a), Fe (b) and Ni–Fe (c) on a glassy carbon works [7,12].
electrode at different values of the electrode potential (V): –0.89 (1);
–0.92 (2); –0.95 (3); –0.98 (4); –1.01 (5); –1.21 (6); –1.23 (7); –1.25
(8); –1.27 (9); –0.86 (10); –0.89 (11); –0.92 (12); –0.95 (13)

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Voprosy Khimii i Khimicheskoi Tekhnologii, 2022, no. 2, pp. 3-8

(i/imax)2 It follows from the observed differences in the

1.2
mechanisms of the initial electrocrystallization
Ni stages of nickel and iron in ethaline that the
1.0
formation of Fe nuclei occurs at a significantly
0.8 lower rate than in the case of Ni. This may be due
to bot differences in the nature of these two
0.6 metals and the conditions under which this
progressive
instantaneous processes occur (differences in the potentials of
0.4 -0.89 V
-0.92 V electrodeposition, surface charge, and structure
-0.95 V
0.2 -0.98 V
and composition of the double layer).
-1.01 V Experimental data on the kinetics of
0.0 electrochemical nucleation of the Ni–Fe alloy
0.0 0.5 1.0 1.5 2.0 2.5
(Fig. 2,c) indicate the implementation of the
t/tmax
mechanism of instantaneous nucleation. Thus, it
a can be argued that during codeposition of these
two metals from ethaline solution on a glassy
(i/imax)2 carbon electrode, nickel imposes on iron not only
1.2 its potential region where deposition occurs, but
Fe also the nature of electrochemical nucleation
1.0
mechanism described by Eq. (1). It is known that
0.8
the mechanism of instantaneous nucleation is
typical of the deposition of alloys–solid solutions
0.6 [15], a typical representative of which is the
progressive
nickel-iron alloy [4,8].
0.4 instantaneous
-1.21 V
0.2 -1.23 V
-1.25 V Conclusions
-1.27 V
0.0 Electrolytic deposition of nickel and iron from the
0.0 0.5 1.0 1.5 2.0 2.5
electrolyte based on deep eutectic solvent
t/tmax
ethaline on the surface of a glassy carbon
electrode obeys the patterns of three-
b
dimensional instantaneous nucleation and
(i/imax)2 progressive nucleation, respectively. The nickel
1.2 component of the alloy imposes its own
Ni-Fe mechanism of instantaneous nucleation during
1.0
electrodeposition of Ni–Fe alloy from ethaline-
0.8
based solution.

0.6
Acknowledgments
progressive
0.4
instantaneous This work was supported by the Ministry of
-0.86 V
0.2 -0.89 V Education and Science of Ukraine (project no.
-0.92 V
-0.95 V 0121U109551).
0.0
0.0 0.5 1.0 1.5 2.0 2.5
t/tmax
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e-mail: [email protected]
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Danilov F.I., Sknar I.V., Sknar Yu.E., Pavlenko model developed by Scharifker and Hills was used to
L.M. // Voprosy Khimii i Khimicheskoi interpret the obtained experimental data. It was shown that
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Keywords: electrochemical crystallization; nickel; iron; alloy;
Received 11.02.2022
deep eutectic solvent.

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Voprosy Khimii i Khimicheskoi Tekhnologii, 2022, no. 2, pp. 3-8

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