Electrodeposition of Ni, Fe and Ni-Fe alloys on a 316 stainless steel surface in a fluorborate bath

Article abstract of DOI:10.1016/j.electacta.2009.05.076

Electrodeposition processes of Ni, Fe and Ni-Fe alloys on 316 stainless steel surfaces in fluorborate baths were studied using conventional electrochemical techniques and atomic force microscopy. The results showed that these processes occurred under mass

Full text of DOI:10.1016/j.electacta.2009.05.076

Electrochimica Acta 54 (2009) 6257–6263
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Electrochimica Acta
journal homepage: www.elsevier.com/locate/electacta
Electrodeposition of Ni, Fe and Ni–Fe alloys on a 316 stainless steel
surface in a fluorborate bath
∗
Chang-wei Su, Feng-jiao He , Hui Ju, Yu-bin Zhang, Er-li Wang
College of Chemistry and Chemical Engineering, Hunan University, Changsha, Hunan 410082, PR China
a r t i c l e i n f o
a b s t r a c t
Article history:
Electrodeposition processes of Ni, Fe and Ni–Fe alloys on 316 stainless steel surfaces in fluorborate baths
were studied using conventional electrochemical techniques and atomic force microscopy. The results
showed that these processes occurred under mass transfer control, associated with nucleation and growth
process. Cathodic current–time transients indicated that the nucleation and growth of Ni–Fe alloy was
different from that of the single metal (Ni or Fe). For one, two nucleation and growth processes occurred
during Ni–Fe alloy codeposition. Also, there was a nucleation and growth process of Ni–Fe alloy on Ni–Fe
clusters, due to a change of the Ni–Fe alloy composition and phase. Homogeneous Ni–Fe alloy deposits
could be obtained by pulse potential plating. AFM images of Ni, Fe and Ni–Fe deposits prepared by pulse
potential plating revealed the following results: (1) the growth rate of Ni nuclei was faster in parallel
than in perpendicular to the 316 electrode surface; (2) for Fe nuclei, the preferential growth direction was
perpendicular to the 316 electrode surface; and (3) for Ni–Fe nuclei, there was no preferential growth
direction and uniformly hemispherical Ni–Fe clusters were obtained.
Received 10 March 2009
Received in revised form 24 May 2009
Accepted 24 May 2009
Available online 6 June 2009
Keywords:
Electrodeposition
Nickel
Iron–nickel alloy
Fluorborate
Nucleation and growth
©
2009 Elsevier Ltd. All rights reserved.
1
. Introduction
An inorganic complexing reagent, fluorboric acid does not
cause problems during the electrodeposition of Ni–Fe alloy [17].
Because it is a strongly corrosive acid, there is very little litera-
ture precedent for Fe group alloy electrodeposition in fluorborate
baths [18]. A fluorborate bath was found to be appropriate for
Due to their magnetic properties and dimensional stability,
Ni–Fe binary alloys have been fabricated by researchers using
different techniques, such as sputtering [1], ball milling [2] and
electroplating [3–14]. Compared with other methods, the elec-
trodeposition method allows for mass production of Ni–Fe alloys
at a low cost. Moreover, it provides the possibility of preparing
Ni–Fe alloys with different structures. For example, Ni–Fe alloys
with nanosized grains can be easily prepared using this method
the continuous deposition system, and bright and flexible Ni1 Fex
−x
(0.1 < x < 0.75) alloys have been prepared by our group in the bath
[17].
In this paper, the electrodeposition processes of Ni, Fe and Ni–Fe
alloys in fluorborate baths were investigated using conventional
electrochemical techniques, such as cyclic voltammetry, current
transients, and anodic linear sweep voltammetry. Atomic force
microscopy (AFM) was employed to analyze the surface microstruc-
ture of the Ni, Fe and Ni–Fe alloys. Because the Ni–Fe deposits could
be easily separated from 316 stainless steel (ss) [20], a 316 ss elec-
trode was selected for the present study. The results will allow
for greater understanding and control over the Ni–Fe codeposition
process.
[
3–6]. Also, this method enhances the properties of the alloys, such
as improved electrical resistivity and hardness, as well as corrosion
resistance [15].
Various Ni–Fe plating bath recipes have been proposed and
reviewed previously in the literature by Andricacos and Romankiw
[
16]. These recipes can be classified into two categories: simple salt
systems [7–11] and complexing reagent systems [12–14]. The com-
plexing reagent bath is more stable, especially at high pH values.
Many complexing reagents, such as citric acid, tartaric acid, glycine,
and sulfamate acid, however, affect and even change the properties
of the Ni–Fe alloy by accumulating their cathodic reaction prod-
ucts during electrodeposition. Thus, this proposed set of baths is
not appropriate for a continuous deposition system.
2. Experimental
The bath composition in the present study is shown in Table 1.
All baths were prepared using pure water (16 Mꢀ cm, prepared by
a Molresearc1005a made in Shanghai by Molecular Biotec. Ltd.)
and analytical grade reagents. The bath pH value was adjusted to
3.0 with the fluorboric acid solution. The bath temperature was
∗ Corresponding author. Tel.: +86 731 8621930; fax: +86 731 8808630.
E-mail address: fengjiao863@hotmail.com (F.-j. He).
◦
maintained at 40 ± 0.2 C with a thermostat.
0
013-4686/$ – see front matter © 2009 Elsevier Ltd. All rights reserved.
doi:10.1016/j.electacta.2009.05.076

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C.-w. Su et al. / Electrochimica Acta 54 (2009) 6257–6263
Table 1
The cyclic voltammogram obtained in the Fe bath is shown in
Chemical composition of the Ni, Fe, and Ni–Fe plating baths.
Fig. 1b. The clear cathodic peak and the corresponding sharp anodic
stripping peak are observed at potentials of −1.15 and −0.55 V,
respectively. Beyond the anodic stripping peak the current rapidly
approaches zero, indicating that the majority of the deposited Fe
has been removed from the substrate surface. Moreover, the plot
during the anodic part of the cycle also crosses over the plot of the
cathodic cycle.
Bath
Ni(BF4)2
Fe(BF4)2
NaBF4
H3BO3
Ni
Fe
Ni–Fe
0.1 M
–
0.075 M
–
1.8 M
1.8 M
1.8 M
0.6 M
0.6 M
0.6 M
0.1 M
0.025 M
The cyclic voltammogram obtained in the Ni–Fe bath, shown in
Fig. 1c, clearly shows that only one cathodic peak occurs, indicating
codeposition of Fe and Ni. Such a wide anodic stripping shoulder
indicates Ni–Fe alloy deposition with successive alloy composition.
In addition, the crossover phenomenon also occurs.
The electrochemical experiments were carried out in a conven-
tional three-electrode cell (100 ml). A 316 stainless steel (ss) disk
electrode with an area of 0.071 cm2 was used as the working elec-
trode. A graphite rod and a saturated calomel electrode (SCE) were
the counter electrode and reference electrode, respectively. Before
electrodeposition, the working electrode was polished to a mirror
with 50 nm alumina powder, sonicated for 5 min in a pure water
bath (16 Mꢀ cm), and rinsed thoroughly with pure water.
Electrochemical measurements were performed using an elec-
trochemical workstation (IM6ex, ZAHNER-elektrik GmbH & Co.
KG, Germany; CHI 660B, Chenhua Instrument Limited Company,
Shanghai). The iron content of the deposits was analyzed using
WFX-1C atomic absorption spectrometry. Surface morphology of
the obtained deposits was characterized by AFM (SPA-400 SEIKO).
These crossover points indicate that the metal deposits more
easily on itself than on the 316 ss.
The influence of the potential scan rate (v) on the Ni, Fe and
Ni–Fe depositions are shown in Fig. 2. In each group of linear sweep
voltammograms, a gradual shift of the cathodic peak toward more
negative values can be seen to occur when the scan rate increases.
Plots of cathodic current value (Ip) versus the square root of the scan
1/2
rate (v ) are shown in Fig. 2d. The linear relationship between Ip
and v1 suggests that these reduction processes occurred under
mass transfer control [21]. The plotted lines did not pass through
the origin, likely due to the effect of the nucleation and growth
process [22,23].
/2
3. Results and discussion
3.1. Voltammetric studies
3.2. Potentiostatic studies
Typical cyclic voltammograms of 316 stainless steel – recorded
3.2.1. Single potential step
in an Ni bath, Fe bath and Ni–Fe bath – are shown in Fig. 1. The
voltammetric scans were conducted in the potential range from
The nucleation models for the Ni, Fe and Ni–Fe alloy electrocrys-
tallization processes on the 316 ss electrode were further studied
by a more convenient potentiostatic technique. An initial potential,
0 V versus SCE, was selected, where no metal deposition occurs
in any of the cyclic voltammograms in Fig. 1. The potential steps
were performed from the initial potential to a negative potential
between −0.85 and −1.25 V. Fig. 3 shows a set of current transients
obtained from different step potentials and at different baths. When
the applied step potential (Es) was more positive than the crossover
−
1
0
to −1.2 V versus SCE at a scan rate of 20 mV s . For the cyclic
voltammogram obtained in the Ni bath, shown in Fig. 1a, the main
features are a sharp cathodic peak centered at −1.07 V in the for-
ward cycle and a crossover between the anodic and cathodic parts
of the voltammetric plot. It is found that the anodic dissolution of
the Ni deposit is strongly suppressed, likely due to passivation of
nickel deposits.
Fig. 1. Cyclic voltammograms obtained on 316 stainless steel electrode in (a) Ni bath; (b) Fe bath; and (c) Ni–Fe bath at scanning rate of 20 mV s−1. The arrows indicate
direction of scan voltages.

C.-w. Su et al. / Electrochimica Acta 54 (2009) 6257–6263
6259
Fig. 2. Linear voltammograms for 316 stainless steel electrode in (a) Ni bath, (b) Fe bath, and (c) Ni–Fe bath at various sweep rates: (1) 10 mV s 1, (2) 20 mV s−1, (3) 50 mV s
and (4) 100 mV s . (d) The relationship of peak current with potential sweep rate in three baths.
−
−1
−1
potential (Ec), Es ≥ Ec + 0.1 V, all transients exhibited a simple plot,
due to a lack of crystallization of the metal at these potentials. The
characteristics of the amperommograms obtained from a more neg-
ative Es than Ec, can be described as follows: (i) a strong falling
current was observed in the initial period of time, corresponding
to the charging of a double layer [24] or other processes [25–27],
such as adsorption [26,27]; (ii) then, a current platform, denoting
an induced period, decreased with the decrease of Es, (iii) next, a
rising current was caused by nucleation and the growth of the Ni,
Fe and Ni–Fe alloys, (iv) subsequently, the current reached a max-
imum (im) and the corresponding time was defined as tm (both im
and tm are dependent on the applied Es), and (v) a decay current was
related with the diffusion of metal ions and then approached a limit
diffusion current. The limit current varies with Es, likely resulting
from a hydrogen evolution reaction (HER) or a change in the surface
morphology.
For single metal deposition, only a current peak appeared (see
Fig. 3a and b). But, for Ni–Fe alloy deposition, a current shoulder
(C ) and a current peak (C ) can be observed in the inset in Fig. 3c,
1
2
appearing at 0.5 and 0.75 s, respectively, in the current transient
Fig. 3. A set of current transients of (a) Ni deposition, (b) Fe deposition and (c)Ni–Fe codeposition at different step potentials indicated in figure. Insets: magnified curves at
short times.

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2
2
Fig. 4. Comparison between non-dimensional plots, i /i vs. t/tm, obtained from (a) Ni bath and (b) Fe bath with the theoretical non-dimensional curves according to Eqs.
m
(
1) and (2).
obtained at −1.2 V. This implies that the second nucleation and
growth process occur during Ni–Fe deposition.
Fig. 4 shows a comparison of the theoretical dimensionless
transients generated by Eqs. (1) and (2), with experimental dimen-
sionless current transients obtained with different baths. The
nucleation mechanisms of Ni and Fe can be distinguished to be pro-
gressive and instantaneous, respectively. The strong falling currents
in the initial period of time may affect the diagnostication of nucle-
ation mechanisms. Some researchers have attempted to eliminate
the effect of the falling currents on the current transients [24–27].
Many models have been proposed [19,28–35] to analyze such
current–time transients. Because Ni and Fe electrodeposition are
controlled by diffusion, a simple Scharifker and Hills (S–H) model
was used to deal with the present current transients [19,36–38]. The
model is not valid for Ni–Fe alloy electrocrystallization, due to the
interaction of Ni and Fe nucleation and growth, or even the occur-
rence of the second nucleation and growth processes during Ni–Fe
electrodeposition. Therefore, the nucleation mechanisms of only
Ni and Fe will be discussed. According to the S–H model, the the-
oretical diagnostic relationship in a non-dimensional form is given
by
2
2
The deviation of the i /i ratio from the S–H model occurs when
m
Es is more positive (such as when Es = −1.0 for Ni deposition) and
the time exceeds tm, probably because of HER [35,39]. Hence, Fig. 4
demonstrates only the approximative results, and the nucleation
and growth models of Ni and Fe need a further discussion.
ꢀ
ꢁ
2
ꢂ
ꢃ
ꢀ
ꢁꢄꢅ
2
i
1.9542
t/tm
t
3
.2.2. Multiple potential steps
Fig. 5 presents multiple step transients obtained from different
=
1 − exp −1.2564
(1)
im
tm
baths. The experiments were conducted by stepping the poten-
tial of the 316 ss from an initial potential to a potential of −1.2 V,
jumping back to the initial potential, and then repeating these two
processes. The pulse width was 0.2 s. According to the cyclic voltam-
mograms in Fig. 1, the initial potentials were selected to be −0.6,
for instantaneous nucleation, and
ꢆ
ꢇ
ꢈꢉ
ꢀ
ꢁ
2
ꢀ
ꢁ
2
2
i
1.2254
t/tm
t
=
1 − exp −2.3367
(2)
im
tm
−
0.7, and −0.7 V for the Ni bath, Fe bath and Ni–Fe bath, respec-
for progressive nucleation.
tively. At these initial potentials, no deposition or stripping currents
Fig. 5. Chronoamperograms of (a) Ni, (b) Fe and (c) Ni–Fe deposition by multiple potential steps.

C.-w. Su et al. / Electrochimica Acta 54 (2009) 6257–6263
6261
Fig. 6. A set of anodic linear sweep voltammograms for (a) Ni deposits, (b) Fe deposits and (c) Ni–Fe deposits obtained in respective bath (shown in Table 1) at the potential
of −1.2 V vs. SCE for seconds indicated in figure.
occurred in the electrolytes. Here, the cathodic current transients
are only discussed; the effect of the charging of the double layer or
other processes has not been taken into account.
It can be observed from Fig. 5a and b that the first two cathodic
current transients rose due to Ni and Fe nucleation on the 316 ss
electrode, the third transient showed a current platform, and then
the followed transients presented only falling currents, implying
that nucleation clusters of single metals depositing on themselves
was not a main contribution to the cathodic current.
metallic alloys [44,45]. Fig. 6 shows a set of ALSVs measured in the
corresponding metal deposition baths after a single potential step
at −1.2 V for several seconds, with a scan rate of 100 mV/s. Since
the baths shown in Table 1 contain the same, high concentration,
supporting electrolyte, the conditions of all the ALSVs can be con-
sidered to be the same. For nickel (Fig. 6a), the anodic stripping
peaks occurred at a potential of −0.1 V versus SCE, and dissolving
−
2
current values were about 1 mA cm . Such a low current means
that the passivation of nickel deposits occurred. For iron (Fig. 6b),
the notable character of the ALSVs was a sharp current peak with
tentimesthecurrentasNi. Thepeakcurrentincreasedwithincreas-
ing step time (deposition time), which indicates that more iron
deposited in the chronoamperometric experiment.
But, for the Ni–Fe multiple transients shown in Fig. 5c, from the
fourth cathodic current transient on, a rising current and even a cur-
rent peak can be observed, indicating that a nucleation and growth
process occurred during Ni–Fe deposition on Ni–Fe clusters. That
is, the growth of Ni–Fe nuclei can be interrupted, and consequently
the crystal size can be controlled by the potential pulse width. Since
metal nucleation usually occurs on a foreign substrate, it is likely
that the alloy composition of the forming Ni–Fe nuclei is different
than that of substrate (Ni–Fe clusters, at least on their surface).
It is well known that Ni deposition is inhibited by iron ions,
resulting in an anomalous codeposition of Ni–Fe [40–43]. That is,
However, it can be observed from Fig. 6c that the shape of the
Ni–Fe ALSVs varies with the deposition time. When the deposition
time is shorter than 0.6 s, the ALSVs present a sharp current peak
that increases with deposition time. For times longer than 0.6 s, the
dissolution peak shifted positively and widened, meaning that the
iron content in the Ni–Fe alloy deposits decreased. The alloy phase
the rate constant (k) of Fe2 to Fe is faster than that of Ni to Ni
during their codeposition. At the initial stage (at very short times),
the metal ion reduction is limited by the kinetic parameter, k, and
not by diffusion. This must result in high iron content in the Ni–Fe
nuclei. Then, the iron content in Ni–Fe deposits decreases due to the
effect of diffusion and approaches a constant controlled by diffu-
sion. As such, Ni–Fe clusters with different iron contents from their
inner to outer were formed. During the off-time period, the Fe2 ion
concentration at the nearby electrode recovered by ion migration.
Therefore, iron content in the forming Ni–Fe nuclei is higher than
that of the surface Ni–Fe clusters; consequently a nucleation and
growth occurs.
+
2+
+
3.3. Anodic linear sweep voltammetry (ALSV)
Fig. 7. A set of anodic linear sweep voltammograms for Ni–Fe deposits obtained by
pulse plating. The pulse width is 0.2 s, and cathode potential is −1.2 V. Pulse periods
are indicated in figure.
ALSV is particularly useful as a simple and easy ‘in situ’ elec-
trochemical method for identifying the phase and composition of

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Fig. 8. AFM images of (a and b) 316 ss electrode; (c and d) Ni deposit; (e and f) Fe deposit; (g and h) Ni–Fe alloy deposit obtained by multiple potential steps. (a, c, e and g)
D images, (b, d, f and h) 3D images. The pulse width is 0.2 s, and cathode potential is −1.2 V. Total time is 20 s.
2

C.-w. Su et al. / Electrochimica Acta 54 (2009) 6257–6263
6263
transition likely occurred between 0.5 and 0.6 s, since the character
of the corresponding ALVSs significantly changed. This period of
time is consistent with that of the onset time of peak C2 shown in
the Ni–Fe current transient at −1.2 V (see the inset shown in Fig. 3c).
This result indicates that the second nucleation and growth process
arises from the alloy phase transition during Ni–Fe codeposition
using a single potential step.
are prone to passivation. The ALSVs of the Ni–Fe alloy indicate that
the alloy composition varied with the deposition time.
Uniformly hemispherical Ni–Fe nanocrystals can be prepared by
pulse potential plating. Homogeneous Ni–Fe deposits can be also
obtained using pulse potential plating.
Acknowledgements
The ALSVs of the Ni–Fe alloy deposits obtained by multiple
potential steps are shown in Fig. 7. A pulse width of 0.2 s was
selected. The shape and change of these ALSVs are similar to that
of the Fe ALSVs, but the dissolution peak has shifted positively
This work was supported by the National Key Technologies R&D
Program, 2006-BAE03B04. This work was also supported by the
YingCai Keji Company Limited.
(
between −0.4 and −0.2 V). This peak potential is consistent with
that of the ALSVs of the Ni–Fe alloy obtained by a short potential
step (<0.6 s). The results indicate that homogeneous Ni–Fe alloy was
obtained.
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In the electrolytes, the ALSVs show that iron deposits can easily
take place during electro-dissolution and that the nickel deposits