Materials Sciences and Applications, 2011, 2, 276-283
doi:10.4236/msa.2011.24036 Published Online April 2011 (http://www.scirp.org/journal/msa)
Contribution to a Comparative Study of the
Corrosion Inhibiting Effect of Some Azoles, to
Protect the Cu70-30Ni Alloy in Aerated NaCl 3%
in Presence of Ammonia
Mohammed Benmessaoud1,3, Karima Es-salah1,2,, Ahmed Kabouri3, Najjat Hajjaji1, Hisai Takenouti2,
Abdelah Srhiri1
1Laboratory of Electrochemistry, Materials and Environment (LEME), Faculty of Sciences, Ibn Tofail University, Kenitra, Morocco;
2CNRS UPR 15, LISE, UPMC University, Paris, France; 3University of Mohammed V Agdal, Energy Systems Laboratory, Materials
and Environment, High School of Technology, Salé Medina, Morocco
Received November 20th, 2010; revised January 17th, 2011; accepted March 11th, 2011.
ABSTRACT
Some azoles were tested such as 3-amino-1,2,4-triazole (ATA), 3-4’-bitriazole -1,2,4 (BiTA)and 2-Mercaptobenzimi-
dazole (MBI) against Cu-30Ni alloy corrosion in 3%NaCl polluted by ammonia using potentiodynamic measurements
and electrochemical impedance spectroscopy and non-electrochemical techniques (scanning Electron Microscopy
(SEM)) studied surface morphology has been used to cha racterize electrode surface. This study permitted to follo w the
evolution of the inhibitory effect of some azoles, on Cu-30Ni alloy corrosion in 3% NaCl polluted by ammonia and in-
dicate that the tested inhibitors act as a good mixed-type inhibitor retarding the anodic and cathodic reactions. An in-
crease of the inhibitors concentration lea ds to a decrease of corrosion rate and inhibition efficiency increase.
Keywords: Cu-30Ni Alloy, Electrochemical Impedance Spectroscopy, Ammonia, Inhibition, Azole
1. Introduction
Organic inhibitors are largely used with success to pro-
tect copper and copper alloys against corrosion. Many
papers reported that heterocyclic compounds, such as
azole, reveal marked inhibition efficiency [1-12]. In a
neutral chloride medium, Otmacic and Stupnišek-Lisac
examined the inhibiting effect of non-toxic imidazoles
derivatives, and showed that those containing phenyl
groups showed a better performance [7]. El Issami et al.
studied the inhibiting effect of triazoles (triazole,
amino-triazole and diamino-triazole) in hydrochloric acid,
and they found that the diamino-triazole has the best
performance [8]. For substituted uracils with two azole
radicals, the grafting of thiol groups increased substan-
tially the inhibiting effect [9]. Huynh et al. examined the
alkyl esters of carboxybenzotriazole in sulphate medium
at different pH. In weakly acidic to neutral solutions,
they stated the formation of polymeric complex that hin-
ders corrosion of copper [10]. Laachach et al. confirmed
also that 3-amino-1,2,4-triazole (ATA) exhibits an ex-
cellent protective effect on the corrosion of Cu-30Ni in
NaCl solution because of the complex film with copper
oxide and triazoles formed at the metal surface increases
its stability [11,12]. These experiments were performed
in the absence of pollutants on copper electrode.
Es-Salah et al. examined the inhibiting effect of ATA
and Bitriazole (BiTA) on the corrosion of Cu-30Ni alloy
in 3% NaCl in presence of ammoniac, and they found
that when the ATA and BiTA were added in the solution,
a remarkable inhibiting effect was observed when its
concentration is higher than 1 mM [13,14]. 2-Mercaptoben-
zimidazole (MBI), as an inhibitor, has been studied on
the inhibition of mild steel in sulphuric acid solution [15],
steel in hydrochloric acid [16,17], copper and its alloys in
hydrochloric acid [18], mild steel in phosphoric acid
[19].
Cu-Ni alloys are frequently employed in marine ap-
plications. Al-Hachem and Carew studied the influence
of pollutants such as chlorine and ammonia at low con-
centration (5 ppm) in natural seawater. Both ammonia

Contribution to a Comparative Study of the Corrosion Inhibiting Effect of Some Azoles, to Protect the Cu70-30Ni
Alloy in Aerated NaCl 3% in Presence of Ammonia
277
and chlorine increase slightly the corrosion rate of
Cu-30Ni [20]. Macdonald et al. [21,22] investigated the
corrosion of this alloy in the deoxygenated seawater in
presence of sulphide. They showed that the presence of
sulphide accelerates the corrosion rate of this alloy. In
contrast, Syrett et al. [23] showed that sulphide increased
the corrosion rate in presence of oxygen only. Other au-
thors [24-26] studied the effect of ammoniac. They re-
marked that this pollutant favours a selective dissolution of
Cu-Ni alloys through the formation of copper complexes.
In fact, copper-ammoniac complexes make unstable the
surface layer constituted of corrosion products, which
generally protect the alloy against the corrosion [27,28].
The present investigation discusses the results ob-
tained in studying the inhibiting effect of 2-Mercaptoben-
zimidazole (MBI), 3-4’-bitriazole -1,2,4 (BiTA) and
3-amino-1,2,4-triazole (ATA), against Cu-30Ni alloy cor-
rosion in 3% NaCl polluted by ammoniac. The tested
compounds are presented in Figure 1.
2. Experimental Conditions
A classic electrochemical cell with three-electrode con-
figuration was used in this study: a platinum grid as a
counter electrode, a rotating disk of Cu-30Ni as working
electrode, and Ag/AgCl in 3 M KCl (SSE) as a reference
electrode. All potentials in this paper are referred to this
later electrode.
The working electrode was made of cylinder rod of
Cu-30Ni (Goodfellow) of 12.5 mm in diameter. A cylin-
der rod of about 1 cm height was fixed to a stainless-steel
shaft, and then the lateral part was covered with a cata-
phoretic epoxyamine base paint (PPG; WT724 + P962).
First, the paint was deposited at a constant voltage of 180
V during 4 min, and then cured at 180˚C for 30 min. Af-
ter that, the electrode was embedded into an epoxy resin
(Buhler; Epoxycure), and worked out to the cylinder
shape, the outer diameter of which was 21 mm. Only the
cross-section of the alloy rod embedded in the epoxy
resin was used to form a rotating disk electrode. The
cataphoretic coating allowed avoiding any infiltration of
electrolyte between the metal and epoxy resin interface.
Just before each experiment, the electrode surface was
polished by emery-paper up to 1000 grade.
The corrosion test solution was prepared with de-io-
nized water and reagent grade chemicals: 3 wt% NaCl +
0.05 M NH4OH + 0.05 M NH4Cl. The pH of this buffer
solution was 9.25. MBI and ATA (Fluka; Purum) were
used as received without any special reaction or trans-
formation, BiTA was synthesized.
The potentiodynamic measurements were performed
using a PGP201 potentiostat/galvanostat. The electrode
was immersed for 30 min in the test solution in free cor-
N
N
N
H
NH2
3-amino-1,2,4-triazole (ATA)
2-Mercaptobenzimidazole (MBI)
3-4’-bitriazole -1
,
2
,
4
(
BiTA
)
Figure 1. Compounds investigated.
rosion conditions. Impedance (EIS) measurements were
done using an EG & G apparatus (model 6310), with a
frequency interval ranging from 100 kHz to 10 mHz.
The surface morphology of the electrode was exam-
ined with a scanning electron microscope (SEM; Leica
Stereoscan 440).
3. Experimental Results and Discussion
In the context of a study published elsewhere [13], we
limit ourselves here to have the comparative results at
1mM of each inhibitor.
The morphology and corrosion products covering the
electrode surface were first analyzed by SEM in absence
and in presence of examined inhibitors. Then, the kinet-
ics of corrosion inhibition was examined with polariza-
tion curves and electrochemical impedance spectroscopy
(EIS).
3.1. Surface Film Formed upon Cu-30Ni Surface
by Corrosion
Figure 2(a) presents the surface morphology after 24 h
of immersion in ammoniac containing NaCl 3% solution
in absence of inhibitors (reference solution). It can be
seen that the alloy surface is covered by spongy corro-

Contribution to a Comparative Study of the Corrosion Inhibiting Effect of Some Azoles, to Protect the Cu70-30Ni
Alloy in Aerated NaCl 3% in Presence of Ammonia
278
Figure 2. SEM picture of Cu-30Ni electrode surface after 24
h immersion in 3% NaCl pH 9.25 (corrosion test solution),
(a) Blank, (b) ATA, (c) BiTA, (d) MBI.
sion products. In contrast, in presence of inhibitors (Fig-
ures 2(b-d)), almost no corrosion is revealed, and the
grooves due to the initial surface abrasion remain clearly
visible after 24 h immersion. Some precipitates observed
are NaCl crystals appeared because of insufficient sur-
face rinsing. The comparison of these four figures reveals
a marked inhibiting efficiency of inhibitors.
The corrosion rate will be evaluated quantitatively first
by polarization curves then by electrochemical imped-
ance spectra.
3.2. Polarization Curves
Cathodic and anodic polarization curves of Cu-30Ni al-
loy corrosion in 3% NaCl polluted by ammoniac in the
absence and presence of the examined inhibitors, were
plotted after 30 min of immersion time at free corrosion
potential. The effect of the tested inhibitors was studied.
Values of associated electrochemical parameters such a
corrosion potential (Ecorr), cathodic Tafel slop (bc), corro-
sion current density (Icorr) and inhibition efficiencies (E%)
for the tested inhibitors at the concentration 10–3 M are
given in Table 1.
3.2.1. Cathodic Curves
Cathodic curves of Cu-30Ni alloy in aerated 3% NaCl
solution polluted by ammonia, without and with the
tested inhibitors are shown in Figure 3. A small current
peak, at −0.36 V versus Ag/AgCl, can be noticed when
immersed in the reference solution. This peak may cor-
respond to the reduction of corrosion products formed at
the open-circuit conditions before potential sweep [13,29].
In presence of the tested inhibitors we note a decrease of
the current density values in the vicinity of the corrosion
potential and more particularly in presence of MBI. In
the context of a detailed study published elsewhere
[13,14], an increase of the inhibitors concentration leads
to a decrease of corrosion rate, this decrease is accompa-
nied by the disappearance of the peak raised in the ab-
sence of inhibitors. We also note a large domain of line-
arity indicating a modification of the cathodic process
kinetic control.
The corrosion current density was determined by Tafel
extrapolation of the current density-potential curve after
correction for diffusion, by using the following relation
[30,31]:
*
1
111

I
I
I (1)
where:
I: current density at mixed process.
I*: corrected current density.
I1: limited current density.

Contribution to a Comparative Study of the Corrosion Inhibiting Effect of Some Azoles, to Protect the Cu70-30Ni
Alloy in Aerated NaCl 3% in Presence of Ammonia
279
Table 1. Effect of ATA, BiTA and MBI on the electro-
chemical kinetics of Cu-30Ni in 3% NaCl pH 9.2.
Solution bc (mV/dec) Ecorr (mVAg/AgCl) Icorr (A/cm2)E (%)
Blank –267 –298 91.3 -
1 mM BiTA –213 –214 4.5 95
1 mM ATA –198 –217 1.7 98.1
1 mM MBI –158 –195 0.1 99.8
The inhibiting efficiency E in per cent was calculated
according to the following expression:
0
0
100  corr corr
corr
ii
Ei (2)
where 0
corr
i and icorr stand, respectively, to the corrosion
current density without and with inhibitor.
3.2.2. Anodic Curves
In the anodic domain (Figure 4), the addition of the
tested inhibitors to the corrosion test solution decreases
markedly the rate of alloy dissolution. The current peak,
observed at –200 mV in absence of the inhibitors, disap-
pears in the presence of the tested inhibitors.
The anodic curves presents a passive domain that ex-
tends on 350 mV for MBI, which is clearly observed
compared to blank essay. This effect can be explained by
the fact that the product tested act by adsorption on the
surface of the material and contributes to an establish-
ment of anodic film formation. This passivity is broken
with anodic overpressures higher than 160 mV for MBI.
This effect can be allotted to the destruction or the de-
sorption of film formed by the examined inhibitors on the
surface of the electrode.
Comparatively, the study of these obtained results en-
abled us to arise the following observations:
- The tested inhibitors inhibit both the anodic and ca-
thodic process. Their effect as a mixed type inhibitors.
- The classification of these inhibitors according to
their inhibition efficiency obtained from cathodic and
anodic polarizations curves gives:
MBI > ATA > BiTA
These results make it possible to note an important
protective effect of the tested inhibitors against Cu-30Ni
alloy corrosion as of the addition of 1mM.
3.3. Electrochemical Impedance Spectroscopy
(EIS)
Impedance diagrams were plotted to obtain more infor-
mation about the electrochemical process which carried
at the Cu-30Ni electrode in 3% NaCl solution polluted by
ammonia in presence of BiTA, ATA and MBI.
3.3.1. Effect of the Tested Inhibitors
The impedance diagrams in Nyquist plot for different
inhibitors are after 30 min of stabilization period pre-
sented in Figure 5. The high frequency part of imped-
ance is displayed with an enlarged scale in the insert.
Though not clearly separated, these diagrams may be
split into two capacitance loops. However, in contrast to
the case of copper electrode [32], with the working elec-
trode, the addition of inhibitors does not induce a new
time constant, they remained always two. In the context
of a detailed study published elsewhere [14,29], the im-
pedance spectra in absence of inhibitors present two ca-
pacitive loops, the first loop can be attributed to a charge
transfer process.
In the presence of inhibitors, we note that the imped-
Figure 3. Cathodic polarization curves of Cu-30Ni in 3%
NaCl in presence of ammonia (pH 9.25) without and with
the tested inhibitors at the concentration 10–3 M, Ω = 1000
rpm; |dE/dt| = 30 m/Vs.
Figure 4. Anodic polarization curves of Cu-30Ni in 3%
NaCl in presence of ammonic (pH 9.2) without and with the
examined inhibitors at the concentration 10–3 M, Ω = 1000
rpm; |dE/dt| = 30 m/Vs.

Contribution to a Comparative Study of the Corrosion Inhibiting Effect of Some Azoles, to Protect the Cu70-30Ni
Alloy in Aerated NaCl 3% in Presence of Ammonia
280
ance display of the electrode in inhibitors containing the
solution changes in shape and size, other it can be no-
ticed that the impedance modulus increased dramatically
in presence of tested inhibitors. The presence of two ca-
pacitive loops seems to indicate a diffusion contribution
to the beginning of the experiment. At high frequency
loop, it is found that the charge transfer resistance Rt
value increased in presence of the tested inhibitors,
whereas the double layer capacity value found to be de-
creased (Table 2). The decrease in capacity value was
due to the adsorption of inhibitor molecules on the metal
surface and act as barrier to the oxygen diffusion process.
3.3.2. Effect of the Rotation Speed
Figure 6 presents the impedance spectra in presence of
BiTA, ATA and MBI, when the electrode rotation speed is
limited to 200 rpm and 1000 rpm after 30 min of immer-
sion. No marked effect of rotation speed. This confirms the
appearance of a broad tafelien field in the cathodic domain,
when the tested inhibitors were added, on the one hand, and
makes it possible to allot the first loop has a charge transfer
process. As expected from the effect of rotation speed
[13,14,29], the diffusion does not modify the electrode ki-
netics at low cathodic or at the corrosion potentials.
3.3.3. Influence of Time Immersion
Figure 7 shows the impedance diagrams obtained with-
out and with 10–3 M of BiTA, ATA and MBI at the cor-
Table 2. The results of non-linear values regression for the
impedance spectra presented in Figure 5.
Solution Rt (k·cm2) Cd (F/cm2) E’ (%)
Blank 0.450 145 -
1 mM BiTA 7.25 87.2 94
1 mM ATA 11.16 17 96
1 mM MBI 34.5 6.6 97
Table 3. Rt and Cd changes with respect to immersion pe-
riod in the test solution added of 1 mM of BiTA, ATA and
MBI for  = 1000 rpm.
Solution Time (h)Rt k·cm2 Cd F/cm2 E (%)
0.5 0.450 145 -
2 0.372 171 -
4 0.196 123 -
Blank
24 0.177 90.1 -
0.5 4.6 138 90
2 11.5 43 96.7
4 12 46 98.3
1 mM BiTA
24 14 10 98.7
0.5 11.2 17 96
2 17.3 3.3 97.8
4 21.1 5.3 99
1 mM ATA
24 33 1.1 99.4
0.5 34.5 6.6 97.1
2 45.6 3.5 99.2
4 57.6 4.8 99.6
1 mM MBI
24 125 1.3 99.7
Figure 5. Impedance diagrams of Cu-30Ni in the corrosion test solution in absence and presence of BiTA, ATA and MBI af-
ter 30 min of stabilization period. Ω = 1000 rpm; |dE/dt| = 30 m/Vs.

Contribution to a Comparative Study of the Corrosion Inhibiting Effect of Some Azoles, to Protect the Cu70-30Ni
Alloy in Aerated NaCl 3% in Presence of Ammonia
281
Figure 6. Impedance diagrams of Cu-30Ni in the corrosion
test solution in presence of BiTA, ATA and MBI after 30
min of immersion at different rotation speed.
rosion potential after the Cu-30Ni was exposed to the
solution for different times.
The evolution of the characteristic parameters associ-
ated with the capacitive loop with time is summarized in
Table 3. The value of the associated capacity was calcu-
lated from the relation C = 1/(2fRt), where f is the
characteristic frequency in the maximum of the loop and
Rt is the diameter of the first capacitive loop.
The various diagrams of Figure 6 show a capacitive
behavior of the interface in the field of frequency exam-
Figure 7. Impedance diagrams of Cu-30Ni in the corrosion
test solution in presence of 1 mM of tested inhibitors ex-
posed for different times.  = 1000 rpm.
Real part (kOhm·cm2)
Imaginary part (kOhm·cm2)

Contribution to a Comparative Study of the Corrosion Inhibiting Effect of Some Azoles, to Protect the Cu70-30Ni
Alloy in Aerated NaCl 3% in Presence of Ammonia
282
values of polarization resistances can be classified ac
ined. As can be seen in this figure, the impedance dia-
grams in the Nyquist plot become larger with time. The
increase of the polarization resistance with the immersion
period is often reported for the inhibiting action of het-
erocyclic on copper corrosion [5-7,9,10]. However the
cording to an order ascending:
  
p
MBIp ATAp BiTA
RRR
The capacitive behavior seems is not affected with
immersion period. The Cd values observed in presence of
examined inhibitors correspond to those usually allotted
to the double layer.
If we interpret the action of the inhibitors by the varia-
tion of charge transfer resistance Rt,, the inhibition effi-
cien cies evaluated using the following relation:
0
100  
i
tt
i
t
RR
ER (3)
where Rti and Rt0 are respectively charge transfer resis-
tance with and without inhibitor, corroborate those ob-
tained with the stationary curves of polarization.
In the whole cases, the protective effectiveness is
higher than 99%. Furthermore, the inhibiting efficiency
tends to increase with immersion period. Compared with
the solution without ammoniac [11], it was observed that
protective effect of inhibitors is reinforced, and the cor-
rosion current becomes smaller in spite of Cu-NH3 com-
plex formation.
4. Conclusions
The comparative analysis of the results obtained in this
work with the examined inhibitors shows that:
The ATA, BiTA and MBI act at the same time on the
reactions anodic and cathodic of the process of corrosion.
Indeed the cathodic domain is characterized for the ex-
amined inhibitors, by decrease of the current density
values in the vicinity of the corrosion potential and more
particularly in presence of MBI and disappearance of the
cathodic peak, recorded in the absence of inhibitors. The
anodic polarization curves show a decrease of the current
density values with disappearance the current peak re-
corded in the absence of the examined inhibitors. The
values of charge transfer resistances raised of the im-
pedance diagrams show the same evolution in time for all
tested inhibitors, but with different values. The calculated
inhibiting effectiveness remains important for all inhibi-
tors.
The kinetic effect of the tested inhibitors is two-fold:
in one hand, their presence suppresses completely the
oxygen evolution reaction, and merely the hydrogen
evolution reaction is taking place at the electrode surface.
On the other hand, the latter is reduced at least by one
order of magnitude when 1 mM was added into the test
solution. What shows that the use of only one compound
is very sufficient to ensure an important protection of
alloy in the corrosive medium used, that shows that the
use of only one compound can be satisfactory to ensure
an important protection of alloy in the studied corrosive
medium?
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