ISSN: 2319-8753

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Vol. 3 , Issue 3, March 2014

Corrosion Inhibition of Aluminum in

Hydrochloric Acid Solutions Using Some
Chalcone Derivatives
A. S. Fouda*, K. shalabi, N. H. Mohamed
Department of Chemistry, Faculty of Science, El-Mansoura University, El-Mansoura-35516, Egypt

Abstract: The inhibition effect of some Chalcone derivatives [3-(4-hydroxyphenyl)-1-phenylprop-2-en-1-one as an

inhibitor (1) and 3-(4-hydroxyphenyl)-1-(4-nitrophenyl)prop-2-en-1-one as an inhibitor (2)] on the corrosion of
aluminum in 0.5 M HCl solution was studied using potentiodynamic polarization, electrochemical impedance
spectroscopy (EIS), electrochemical frequency modulation (EFM) and weight loss measurements. The results drawn
from the different techniques are comparable and exhibit small discrepancy. Results for weight loss indicated that
inhibitor efficiency (% IE) increased with increasing inhibitor concentration, reaching a maximum inhibiting power of
85.9 , 95.7 % at 21 x 10-6 M for inhibitors 1 and 2, respectively and decreased with increasing the temperature.
Polarization studies clearly revealed that the presence of inhibitors changes the mechanism of hydrogen evolution and
the metal dissolution i.e. they act as mixed type inhibitors. Some activation and adsorption thermodynamic parameters
were calculated and discussed. The surface coverage of the inhibitors obeyed Langmuir adsorption isotherm.

Keywords: Chalcone derivatives, Aluminum, HCl, Potentiodynamic polarization, EIS, EFM, Langmuir
isotherm

I. INTRODUCTION
Aluminum is one of the metals which used in different human activities and many of important applications, where it is
the second most abundant metal after iron, it has a low atomic mass and negative value of standard electron potential,
aluminum potentially attracts as an anodic material for power sources with high energy density. It is used in
construction, packing and transportation because of its strength and electrical conductivity. Aluminum is used in
electronics due to it is super purity [1]. Although Al has an adhesive protective passivating oxide film, but this film has
an amphoteric susceptibility, and consequently the metal dissolves readily in acidic and basic solutions concentrated
above and below pH 4-9 [2, 3]. In our efforts to mitigate electrochemical corrosion of aluminum, the main strategy is to
isolate the metal from corrosive agents and this can be achieved by using corrosion inhibitors which prevent the
adsorption of the aggressive anions or by the formation of a more resistance oxide film on the metal surface. Generally,
it has been assumed that the first stage in the action mechanism of the inhibitors in aggressive acid media as
hydrochloric acid is the adsorption of the inhibitors on the metal surface where HCl solutions are used for pickling of
aluminum for its chemical or electrochemical etching [4]. Various mechanisms have been proposed to explain the
breakdown of the passive oxide film when chloride reach the metal film interface. Recently, has shown that chloride
does not enter the oxide film but it is chemisorbed on the oxide surface [5] and act as a reaction partner, aiding
dissolution via the formation of oxide-chloride complexes. Among several methods used in combating corrosion
problems, the use of chemical inhibitors remains the most cost effective and practical method [6, 7]. From this point of
view, a great number of investigators have conducted research work to find effective inhibitors for aluminum corrosion
in harsh environments [8-10]. Some reported the effect of inorganic oxidants [8], while others studied the use of
organic compounds [11-14]. It is well known that azole derivatives like benzotriazole, mercaptoben, benzimidazole and
imidazole can be employed as inhibitors against corrosion for many metals and alloys. Azole compounds have been
used to protect the corrosion of aluminum [15] in corrosive environments. In general, organic compounds with oxygen,
sulfur, and/or nitrogen as polar groups and conjugated double bonds in their structures have been reported to be good
corrosion inhibitors for many metals and alloys in corrosive media [16–32]. The inhibiting action of these organic
compounds is usually attributed to their interactions with the metallic surfaces via their adsorption. Polar functional

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groups are regarded as the reaction center that stabilitizes the adsorption process [6]. However, the adsorption of an
inhibitor on a metal surface depends on a few factors, such as the nature and surface charge of the metal, the adsorption
mode, the inhibitor’s chemical structure, and the type of the electrolyte solution [33].
In this work, we investigate the effect of some chalcone derivatives on the corrosion behavior of aluminum in 0.5 M
HCl solution using chemical, electrochemical techniques and quantum chemical calculations.

II. EXPERIMENTAL
2.1. Materials and reagents
Aluminum sheets with purity more than 98.8 % were used in this study. The aggressive solution, 0.5 M HCl was
prepared by dilution with bidistilled water. The chalcone derivatives were synthesized according to the procedures
described in previous paper [34] and are presented in Table 1. 10-6 M stock solutions from the investigated compounds
were prepared by dissolving the appropriate weights of the used chemically pure solid compounds in absolute ethanol.

Table 1: structures, molecular weights and molecular formulas of the investigated Chalcone derivatives
Molecular weights &
Names Structures
Chemical formulas

3-(4-hydroxyphenyl)-1- 224.25
1
phenylprop-2-en-1-one C15H12 O2

3-(4-hydroxyphenyl)-1-(4- 269.25
2
nitrophenyl)prop-2-en-1-one C15H11 NO4

2.2. Weight loss measurements

The Seven parallel aluminum sheets of (2.4 x 2.5 x 0.1 cm) were abraded with emery paper (grade uo to1200 grit size)
and then washed with bidistilled water and acetone. After accurate weighing, the specimens were immersed in a 250 ml
beaker, which contained 100 ml of HCl with and without addition of different concentrations of the investigated
compounds. All the aggressive acid solutions were open to air and the measurement was conducted at room
temperature (25 ± 1 °C). After 5 h, the specimens were taken out, washed, dried, and weighed again accurately. The
average weight loss of seven parallel aluminum sheets could be obtained. The inhibition efficiency (% IE) and the
degree of surface coverage, θ, of investigated compounds for the corrosion of aluminum in HCl were calculated as
follows [35]:
% IE = θ x 100 = [(Wo – W)/ Wo] x 100 (1)
where Wo and W are the values of the average weight losses in the absence and presence of the inhibitor, respectively.

2.3. Electrochemical measurements

The experiments were carried out potentiodynamically in three electrode cell. Platinum foil was used as counter
electrode and a saturated calomel electrode (SCE) coupled to a fine Luggin capillary as the reference electrode. The
working electrode was in the form of a square cut from aluminum sheet under investigation and was embedded in a
Teflon rod with an exposed area of 1 cm2. This electrode was immersed in 100 ml of a test solution for 30 min until a
steady state open-circuit potential (Eocp) was attained. The potentiodynamic curves were recorded by changing the
electrode potential from -0.5 to 1.5 V versus SCE with scan rate of 1 mV/s. All experiments were carried out in freshly
prepared solution at room temperature (25oC) using a thermostat. % IE and the degree of surface coverage (θ) were
calculated from Eq. (2):

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%IE =  x 100 = [ 1 – (icorr(inh) / icorr) ] x 100 (2)

where (icorr, and icorr(inh) ) are the uninhibited and inhibited corrosion current density values, respectively, determined by
extrapolation of Tafel line.
The electrochemical impedance spectroscopy (EIS) spectra were recorded at open circuit potential (OCP) after
immersion the electrode for 30 min in the test solution. The ac signal was 5 mV peak to peak and the frequency range
studied was between 100 kHz and 0.1 Hz. The main parameters deduced from the analysis of Nyquist diagram are the
polarization resistance Rp and the capacitance of double layer ( Cdl) which is calculated from Eq.(3):
Cdl =1/ (2 π fmax RP ) (3)
where (fmax) is the angular frequency at which the imaginary component of the impedance reaches its maximum values.
The inhibition efficiency (%IE) and the surface coverage (θ) of the used inhibitors obtained from the impedance
measurements were calculated by applying the following relations:
% IE = θ x 100 = [1- (Rp° /Rp)]×100 (4)
Where Rpo and Rp are the polarization resistance in the absence and presence of inhibitor, respectively.
Electrochemical frequency modulation (EFM) is a non-destructive corrosion measurement technique that can directly
give values of the corrosion current without a prior knowledge of Tafel constants. Like EIS, it is a small signal ac
technique. Unlike EIS, however, two sine waves (at different frequencies) are applied. The intermodulation spectra
contain current responses assigned for harmonically and intermodulation current peaks. The larger peaks were used to
calculate the corrosion current density (icorr), the Tafel slopes (βc and βa) and the causality factors CF-2& CF-3 [36,37] .
The electrode potential was allowed to stabilize for 30 min before starting the measurements. All the experiments were
conducted at 25± 1°.
All electrochemical measurements were carried out using Potentiostat /Galvanostat/ Zra analyzer (Gamry PCI300/4). A
personal computer with DC105 software for potentiodynamic, EIS300 software for EIS and EFM140 software for EMF
and Echem Analyst 5.21 was used for data fitting.

2.4. Surface morphology

For morphological study, surface features (2.0 cm x 2.0 cm x 0.15 cm) of aluminum were examined before and after
exposure to 0.5 M HCl solutions for 24 hour with and without inhibitor. JEOL JSM-5500 scanning electron microscope
was used for this investigation.

III. RESULTS AND DISCUSSION

3.1. Weight loss measurements
Weight The corrosion rate of aluminum as a function of time and temperature were investigated. Fig (1) represents the
weight loss-time curves in the absence and presence of different concentrations of inhibitor (2) at 25°C (the more
effective inhibitor). Similar curves were obtained for the other inhibitor (not shown). It is obvious that the uniformity
and non-linearity of the plot in the absence of inhibitor suggest that the aluminum corrosion in HCl is a heterogeneous
process involving several steps. Similar observations have been reported for aluminum corrosion in other media [38].
The corrosion of aluminum in HCl in the presence of inhibitor shifted to more uniform and more linear plots, and is
much lower than in case of absence of inhibitor. The inhibition efficiency (% IE) and the surface coverage (θ) that
represents the weight of the metal surface covered by inhibitor molecules were shown in Tables (2). The %IE increases
with increasing the inhibitor concentration indicated that more inhibitor molecules are adsorbed on the metal surface
thus providing wider surface coverage. The optimum concentration required to achieve an efficiency of 95.75% and
85.88% was found to be 21x10-6 M for inhibitors 1 &2, respectively.

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B la n k
-6
1x 10 M
-6
0 .3 2 5X 1 0 M
-6
9X 1 0 M
0 .3 0 -6
13 X 1 0 M
0 .2 8 -6
17 X 1 0 M
0 .2 6 21 X 1 0 M
-6

0 .2 4
0 .2 2
weight loss (mg.cm )
-2

0 .2 0
0 .1 8
0 .1 6
0 .1 4
0 .1 2
0 .1 0
0 .0 8
0 .0 6
0 .0 4
0 .0 2
0 .0 0
50 100 150 200 2 50 3 00
t im e ( m in )
Fig. 1: Weight loss- time curves for aluminum corrosion at different concentrations of inhibitor (2) after 180 min immersion in 0.5 M HCl at 25ºC

Table 2: Inhibition efficiency (% IE) and surface coverage (Ɵ) at different concentrations chalcone derivatives for the corrosion of aluminum after
180 min immersion in 0.5 M HCl at 25ºC

Inhibitor (1) Inhibitor (2)

Concentration,
M
% IE Ɵ % IE Ɵ
1X10-6 67.54 0.6754 72.7 0.727
5X10-6 73.53 0.7353 76.0 0.760
9X10-6 75.66 0.7566 79.1 0.791
13X10-6 76.95 0.7695 85.7 0.857
17X10-6 79.41 0.7941 92.8 0.928
21X10-6 85.88 0.8588 95.7 0.957

3.2. Adsorption isotherms

Corrosion inhibitors are found to protect aluminum corrosion in acid solutions by adsorbing themselves on aluminum
surface where the adsorption of the organic molecules occurs as the interaction energy between molecule and metal
surface is higher than that between the water molecules and the surface [39], and it is regarded as substitution
adsorption process between the organic molecules in the aqueous phase (orgaq) and the water molecules adsorbed on
the aluminum surface (H2O)ads [40].
xH2Oads + Orgsol ↔ Orgads + xH2O (5)
where x is the size ratio, that is, the number of water molecules replaced by one organic molecule. Inhibitors molecules
are either physically or chemically adsorbed on a corroding metal surface, where the physisorbed molecules retard
metal dissolution by inhibiting the cathodic reaction whereas chemisorbed molecules inhibit the anodic reaction by
reducing the inherent reactivity of the metal at the adsorption sites [41]. It was found that the best suitable adsorption
isotherm for the studied inhibitors on the aluminum surface is the Langmuir equation [42] which was defined as
follows:
C/Ɵ = 1/Kads + C (6)
where Kads is equilibrium constant of adsorption process, and C is concentration of inhibitor. The plot of C/Ɵ versus C
for the inhibitors are shown (Figs. 2a,2b) to be linear with slope near unity, and correlation coefficients near to unity in
order to obtain the isotherm. The thermodynamic adsorption parameters were calculated. The well-known
thermodynamic adsorption parameters are the standard free energy of adsorption (∆G°ads), the heat of adsorption
(∆H°ads) and the entropy of adsorption (∆S°ads). These quantities can be calculated by various mathematical methods
depending on the values of Kads from adsorption isotherms at different temperatures [43]. The ∆G°ads can be calculated
from Eq. (7):
Kads = (1/55.5) exp (-∆G°ads / RT) (7)

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where 55.5 is the concentration of water in mol l-1, R is the universal gas constant, and T is the absolute temperature.
(∆H°ads), (∆S°ads) can be calculated from Eqs (8 &9):
Log Kads= (∆H°ads / 2.303RT) + constant (8)
∆G°ads = ∆H°ads - T∆S°ads (9)
Table (3) shows all the estimated thermodynamic adsorption parameters for the chalcone derivatives on aluminum
surface, and concluded that: Large values of Kads mean good inhibition efficiency of the inhibitors and strong electrical
interaction between the adsorbate and the adsorbent. The sign of ∆G°ads was negative which reflects that the adsorption
of these inhibitors is spontaneous process. It is well known that values of ΔG˚ads of the order of 40 kJ mol-1 or higher
involve charge sharing or transfer from the inhibitor molecules to metal surface to form coordinate type of bond
(chemisorption); those of order of 20 kJ mol-1 or lower means that the electrostatic interaction between metal surface
and charged organic molecules in the bulk of the solution indicate a physisorption [44, 45]. The calculated ΔG˚ads
values are above 40 kJ mol-1 which indicate that the adsorption mechanism of the investigated compounds on
aluminum in 0.5 M HCl solution is a chemisorption and shifted to physisorption by increasing temperature, so it is a
comprehensive adsorption (physical and chemical). ∆G°ads values increase (become less negative) with an increase in
temperature which indicate that the adsorption process is an exothermic process. The negative sign of ∆H°ads indicates
that the adsorption process of both inhibitors molecules is an exothermic process. Generally, an exothermic adsorption
process suggests either physisorption or chemisorption while endothermic process is attributed to chemisorption [46].
Generally, enthalpy values up to 41.9 kJ.mol-1 are related to physisorption while those around 100 kJ.mol-1 or higher
are attributed to chemisorption. The unshared electron pairs in investigated molecules may interact with p-orbital of
aluminum to provide chemisorbed film.The values of ∆S°ads are large and negative that is accompanied with
exothermic adsorption process.
0.000030

0.000025

0.000020
25 C, R=0.99157
0.000015 45 C, R=0.97028
C/ 

0.000010

0.000005

0.000000

0.000000 0.000005 0.000010 0.000015 0.000020 0.000025

C, M
Fig. 2.a Langmuir adsorption isotherm of inhibitor (1) on aluminum surface in 0.5 M HCl at different temperatures

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0.000025

0.000020

0.000015
25  C, R=0.9880
C/ 

0.000010
45  C, R=0.9967

0.000005

0.000000

0.000000 0.000005 0.000010 0.000015 0.000020 0.000025

C, M
Fig. 2.b Langmuir adsorption isotherm of inhibitor (2) on aluminum surface in 0.5 M HCl at different temperatures
Table (3) Thermodynamic parameters for the adsorption of inhibitors on aluminum surface in 0.5 M HCl at different temperatures
Inhibitor - ΔG˚ads, -ΔH˚ads , -ΔS˚ads,
Kads x10-3
Temp, °C kJ mol-1 kJ mol-1 J K-1 mol -1
M-1
25 1040.6 44.29 52.42 27.30
1
45 275.0 43.74 52.42 27.30
25 759.2 43.50 60.92 58.46
2
45 1195.2 42.62 60.92 57.55

3.3. Effect of temperature

The importance of temperature variation in corrosion study involving the use of inhibitors is to determine the mode of
inhibitor adsorption on the metal surface. Recently, the use of two temperatures to establish the mode of inhibitor
adsorption on a metal surface has been reported and has been found to be adequate. Thus, the influence of temperature
on the corrosion behavior of aluminum in 0.5 M HCl in the absence and presence of the investigated compounds by
hydrogen evolution method at 25 and 45 °C. Therefore, in examining the effect of temperature on the corrosion
process, the apparent activation energies (Ea) were calculated from the Arrhenius equation [47].
Log (k2 corr / k1 corr) = (Ea /2.303R) x (1/T1 -1/T2) (10)
where k1corr and k2corr are the corrosion rates at temperature T1 and T2, respectively. An estimate of heat of adsorption
was obtained from the trend of surface coverage with temperature as follows [48]:
Qads = 2.303R [log (Ɵ2/1- Ɵ2) – log (Ɵ1/1- Ɵ1)] x (T1 T2 / T2 - T1) (11)
where Ɵ1 and Ɵ2 are the degrees of surface coverage at temperatures T1 and T2, The calculated
values for both parameters are given in Table 4. Increased activation energy (Ea) in inhibited solutions compared to the
blank suggests that the inhibitor is physically adsorbed on the aluminum metal surface [49]. It is seen from Table 4 that
Ea values rose with increasing the inhibitor concentration, suggesting strong adsorption of the investigated inhibitors on
the aluminum metal surface. It has been suggested that adsorption of an organic inhibitor can affect the corrosion rate
by either decreasing the available reaction area (geometric blocking effect) or by modifying the activation energy of the
anodic or cathodic reactions occurring in the inhibitor-free surface in the course of the inhibited corrosion process [50]
The negative sign Qads values indicate that the adsorption process and the degree of surface coverage decreased with
increasing in temperature, supporting the physisorption mechanism [51].

Table 4: The activation energy (Ea) and the heat of adsorption (Qads ) for aluminum dissolution in 0.5 M HCl in the absence and presence of inhibitors
at 25 and 45°C

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Inhibitor (1) Inhibitor (2)

Concentration, Ea, -Qads Ea, -Qads

M kJ mol-1 kJ mol-1 kJ mol-1 kJ mol-1

Blank 49.97 ------ 49.97 ------

1x10-6 70.85 37.01 50.84 1.22
5x10-6 72.46 35.27 52.89 3.85
9x10-6 71.68 32.32 54.10 5.36
13x10-6 69.07 27.25 60.09 12.03
17x10-6 58.63 11.25 83.90 38.31
21x10-6 70.61 29.71 96.91 51.24

3.5. Potentiodynamic polarization measurements

The potentiodynamic polarization curves of aluminum in 0.5 M HCl solutions containing different concentrations of
investigated compounds at 25°C are shown in Figs. (3.a, 3.b) for inhibitors 1, 2 respectively. The corrosion kinetic
parameters such as corrosion current density (icorr), corrosion potential (Ecorr.), the anodic Tafel slopes (βa) and cathodic
Tafel slope (βc), degree of surface coverage (Ɵ) and the inhibition efficiency (%IE) of both inhibitors are shown in
Table 5 for the aluminum in 0.5 M HCl solution in the absence and presence of different concentrations of the both
inhibitors are listed in Table 5. The results of this Table indicated that the corrosion current density (icorr) decreases in
the presence of inhibitors compared to the blank solution and also with increasing the inhibitors concentrations which
suggest that the presence of these compounds retard the dissolution of aluminum in 0.5 M HCl solution. Presence of
these inhibitors cause decrease in the corrosion rate, so shift both the anodic and cathodic curves to lower values of
current densities. This implies that both the hydrogen evolution and the anodic dissolution of aluminum metal are
inhibited. This due to adsorption of the inhibitors over the corroding surface [52, 53]. The slopes of the anodic and
cathodic Tafel lines (βa, βc) were slightly changed on increasing the concentration of the investigated compounds. This
means that there is no change of the mechanism of the inhibition in presence and absence of inhibitors and that
inhibitors affects both anodic and cathodic reactions, so it is mixed type inhibitors. Inhibition efficiency (%IE) was
calculated from equation (2). The order of % IE was found to decrease in the following sequence: inhibitor 2 ˃
inhibitor 1.

0.1

0.01 blank
-2

-6
1x10 M
log i, mA cm

-6
5x10 M
1E-3 -6
9x10 M
-6
13x10 M
-6
17x10 M
1E-4 -6
21x10 M

1E-5

-1.5 -1.0 -0.5 0.0 0.5 1.0

E, V vs. SCE
Fig. 3a: Potentiodynamic polarization curves for the corrosion of aluminum in 0.5 M HCl in the absence and the presence of various concentrations
of inhibitor (1) at 25° C

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0 .1

b lan k
-6
0.0 1 1 x1 0 M
-6
5 x1 0 M
-2
log i, mA cm

-6
9 x1 0 M
-6
1 E -3 1 3 x10 M
-6
1 7 x10 M
-6
2 1 x10 M
1 E -4

1 E -5
-1.5 -1.0 -0.5 0 .0 0 .5 1 .0
E , V vs. S C E
Fig. 3b: Potentiodynamic polarization curves for the corrosion of aluminum in 0.5 M HCl in the absence and the presence of various concentrations
of inhibitor (2) at 25° C

Table 5: Potentiodynamic polarization parameters for the corrosion of aluminum in 0.5 M HCl in the absence and presence of different
concentrations of investigated compounds
Conc., -Ea, mV vs. βa, βc , CR
Inh. i corr , mA cm-2 -1 -1 Ɵ % IE
M SEC V dec V dec mmy-1
Blank 0.0 724 222.00 4.30 8.27 2451 ------ -----
1x10-6 724 99.06 4.00 9.52 940 0.5550 55.50
5x10-6 723 69.43 3.03 8.91 881 0.6881 68.81
-6
(1) 9x10 722 47.30 2.55 3.78 598 0.7280 72.80
13x10-6 725 42.85 1.50 6.26 442 0.8075 8.75
17x10-6 713 38.20 0.89 1.03 166 0.8284 82.84
21x10-6 734 23.51 0.48 1.46 102 0.8944 89.44
1x10-6 721 65.33 2.18 4.8 518 0.8752 87.52
5x10-6 697 54.00 0.88 2.39 463 0.9387 93.87
9x10-6 744 47.37 0.05 0.24 312 0.9562 95.62
(2) -6
13x10 745 36.64 0.05 0.25 202 0.9687 96.87
17x10-6 747 21.06 0.04 0.21 187 0.9811 98.11
21x10-6 749 6.12 0.06 0.25 149 0.9902 99.02

3.6. Electrochemical impedance spectroscopy (EIS) measurements

The corrosion behavior of aluminum in 0.5 M HCl solution in the absence and presence of different concentrations of
the inhibitors was investigated by the EIS method at 25°C after 30 min of immersion. Figs. (4.a, 4.b) show the Nyquist
plot for aluminum in 0.5 M HCl solution in the absence and presence of different concentrations of investigated
compounds. The fact that impedance diagrams have an approximately semi-circular appearance shows that the
corrosion of aluminum in 0.5 M HCl is controlled by a charge transfer resistance process. Small distortion was
observed in some diagrams, this distortion has been attributed to frequency dispersion [54] as a result of surface
roughness, impurities, dislocations, grain boundaries, adsorption of inhibitors and formation of porous layers and
inhomogeneity of the electrode surface. The electrical equivalent circuit model which describes the metal / electrolyte
interface of the present corroding system is shown in Fig. 5. The model consists of the solution resistance (Rs), the
charge-transfer resistance of the interfacial corrosion reaction (Rct), and the double layer capacitance (Cdl). Table 6
shows the EIS data where the Cdl values decrease and the Rct values increase with the increase of the inhibitor
concentrations. This is due to the gradual replacement of water molecules by the adsorption of the inhibitor molecules

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on the metal surface, and decreasing the extent of dissolution reaction. The high (Rct) values are generally associated
with slower corroding system [55, 56]. The decrease in the Cdl can result from the decrease of the local dielectric
constant and/or from the increase of thickness of the electrical double layer [57] suggested that the inhibitor molecules
function by adsorption at the metal/solution interface. The % IE obtained from EIS measurements are close to those
deduced from polarization method. The order of inhibition efficiency obtained from EIS measurements is as follows:
inhibitor 2 ˃ inhibitor 1

Fig. 4: Electrical equivalent circuit used to fit the impedance data

B la n k
-6
1x10 M
35 -6
5X 10 M
-6
30 9X 10 M
-6
25 13X 10 M
-6
17X 10 M
20 -6
21X 10 M
15
(ohm cm )
-2

10
5
0
image

-5
Z

-10
-15
-20
-25
0 20 40 60 80 100
-2
Z re a l (o h m c m )

Fig. 4a: Nyquist plots for the corrosion of aluminum in 0.5 M HCl in the absence and the presence of different concentrations of inhibitor (1) at 25° C

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B la n k
-6
1x10 M
-6
5X 10 M
100 9X 10 M
-6

-6
13X 10 M
-6
17X 10 M
-6
50 21X 10 M
(ohm cm )
-2

0
image
Z

-5 0

-1 0 0
-5 0 0 50 100 150 200 250 300 350 400
-2
Z re a l ( o h m c m )

Fig. 4b: Nyquist plots for the corrosion of aluminum in 0.5 M HCl in the absence and the presence of different concentrations of inhibitor (2) at 25° C

Table 6: Electrochemical kinetic parameters obtained from EIS technique for the corrosion of aluminum in 0.5 M HCl at different concentrations of
investigated compounds at 25°C
Comp. Conc., Cdlx10-5, Rct , Ɵ % IE
M μF cm-2 Ω cm2
Blank 0.0 40.30 2.28 ------- ------
1x10-6 40.00 5.84 0.6094 60.94
5x10-6 34.00 8.27 0.7244 72.44
1 9x10-6 23.90 10.75 0.7880 78.80
13x10-6 13.20 12.49 0.8174 81.74
17x10-6 12.50 16.17 0.8590 85.90
21x10-6 12.40 19.30 0.8819 88.19
-6
1x10 39.40 7.30 0.6875 68.75
5x10-6 37.00 9.05 0.7481 74.81
9x10-6 35.70 11.97 0.8095 80.95
2 -6
13x10 34.10 20.48 0.8887 88.87
-6
17x10 32.60 52.78 0.9568 95.68
21x10-6 21.10 205.40 0.9889 98.89

3.7. Electrochemical frequency modulation (EFM) measurements

The EFM is a nondestructive corrosion measurement technique that can directly give values of the corrosion current
without prior knowledge of Tafel constants. It is generally accepted that in most cases, the corrosion rates determined
with the EFM technique, are much higher than the values determined with other techniques exhibiting low corrosion
rates (58). The modulation frequencies that are used in the EFM technique are in the capacitive region of the impedance
spectra. However, results of the EFM technique showed good agreement of corrosion rates obtained with the Tafel
extrapolation method. Figs. 5 are example of aluminum immersed in 0.5 M HCl solutions and in presence of 21 x10-6 M
inhibitor (2) as an example at 25°C. Each spectrum is a current response as a function of frequency. Table 5 shows the
calculated corrosion kinetic parameters at different concentrations of the investigated compounds in 0.5 M HCl at 25°C
(icorr, βa, βc, CF-2, CF-3 and % IE). From Table 4, the corrosion current densities decrease by increasing the
concentration of investigated compounds and the efficiency of inhibition increases by increasing investigated
compounds concentrations. The causality factors in Table 7 are very close to theoretical values, which according to
EFM theory [59] should guarantee the validity of Tafel slopes and corrosion current densities. Values of causality
factors in Table 7 indicate that the measured data are of good quality. The standard values for CF-2 and CF-3 are 2.0

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and 3.0, respectively. The deviation of causality factors from their ideal values might be due to the perturbation
amplitude which was too small or that the resolution of the frequency spectrum is not high enough. Another possible
explanation is that the inhibitor is not performing very well. The obtained results showed good agreement of corrosion
kinetic parameters obtained with the EFM, Tafel extrapolation and EIS methods.

Table 7: Electrochemical kinetic parameters obtained by EFM technique for aluminum in 0.5 M HCl solutions containing various concentrations of
the investigated compounds at 25 °C
icorr, βa βc CR
Concentration, CF-2 CF-3 θ % IE
µA cm-2 mV dec-1 mV dec-1 mpy
M
Blank 930.30 142 446 560.4 1.5 2.23 -- --
1x10-6 361.70 27.90 89.40 156.9 1.9 2.6 0.6112 61.12
5x10-6 223.10 20.30 26.70 96.77 1.7 3.2 0.7202 72.02
9x10-6 221.71 19.70 26.80 96.01 2.8 3.2 0.7420 74.20
(1)
13x10-6 215.92 20.00 24.30 93.63 1.6 2.4 0.7679 76.79
17x10-6 214.71 19.70 24.10 93.12 1.5 3.1 0.7692 76.92
21x10-6 210.81 20.40 21.90 91.40 2.1 3.1 0.7734 77.34
1x10-6 269.41 67.30 94.60 116.80 1.16 3.48 0.7104 71.04
5x10-6 252.02 71.20 99.60 109.30 1.01 2.48 0.7291 72.91

(2) 9x10-6 233.97 22.80 27.70 139.40 2.87 3.28 0.7485 74.85
13x10-6 215.55 19.80 24.40 129.80 1.77 2.99 0.7683 76.83
17x10-6 166.43 36.50 54.80 72.15 1.63 3.01 0.8211 82.11
21x10-6 78.89 63.60 116 46.98 1.59 3.23 0.9152 91.52
Blank
1E-3

1E-4
log I, A cm-2

1E-5

1E-6

1E-7

1E-8

-0.2 0.0 0.2 0.4 0.6 0.8 1.0 1.2 1.4 1.6

Freq, Hz

1x10-6 M 5x10-6 M
1E-3 1E-3

1E-4 1E-4
log I, A cm-2

log I, A cm-2

1E-5 1E-5

1E-6 1E-6

1E-7 1E-7

1E-8 1E-8

-0.2 0.0 0.2 0.4 0.6 0.8 1.0 1.2 1.4 1.6 -0.2 0.0 0.2 0.4 0.6 0.8 1.0 1.2 1.4 1.6

Freq, Hz Freq, Hz

9x10-6 M 13x10-6 M
1E-3 1E-3

1E-4 1E-4
log I, A cm-2

log I, A cm-2

1E-5 1E-5

1E-6 1E-6

1E-7 1E-7

1E-8 1E-8

-0.2 0.0 0.2 0.4 0.6 0.8 1.0 1.2 1.4 1.6 -0.2 0.0 0.2 0.4 0.6 0.8 1.0 1.2 1.4 1.6

Freq, Hz Freq, Hz

17x 10-6 M 21x10-6 M

1E-3
1E-3

1E-4
1E-4
log I, A cm-2

1E-5
log I, A cm-2

1E-5

1E-6 1E-6

1E-7 1E-7

1E-8 1E-8

-0.2 0.0 0.2 0.4 0.6 0.8 1.0 1.2 1.4 1.6 -0.2 0.0 0.2 0.4 0.6 0.8 1.0 1.2 1.4 1.6

Freq, Hz Freq, Hz

Fig. 5: Intermodulation spectrum for aluminum in 0.5 M HCl solutions without and with various concentrations of compound (2) at 25 ° C

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3.7.2. SEM Characterization

Figure 6 shows the scanning electron microphotographs of aluminum in HCl in the presence of 21 x10-6 M of
investigated compounds. As cn be seen from this Figure, there are distinct differences between the the four aluminum
sheets after the corrosion in acid solution. As for bar aluminum , the surface was seriously damaged as a great deal of
deep cavities and drawbach were found. Under the same corrosion circumstance, the surface of aluminum was smooth
with a few small notches. The phenomenon implied that the presence of inhibitors films can protect the aluminum from
corrosion effictently. On comparing these microphotographs, it appears that maximum smoothing of the surface of test
materials has been observed in presence of compound (2) followed by compound (1). This observation is in conformity
with the observed inhibition efficiency values as discussed earlier.

Free metal metal with acid

In presence of inhibitor I In presence of inhibitor II

Fig. 6: SEM photograph of aluminum for free metal, in absence of inhibitors, and presence of 21 x 10-6 M inhibitors 1 & 2

3.7 Mechanism of Corrosion Inhibition

In general, these inhibitors may be adsorbed on aluminum surface in their neutral or protonated forms (cationic form).
Since it is well known that the aluminum surface is negatively charged in acid solution [60], it is easier for the
protonated molecules to approach the negatively charged aluminum surface due to the electrostatic attraction. In case of
adsorption, this involves the displacement of water molecules from the aluminum surface and sharing electrons
between the hetero-atoms and aluminum. Also, the inhibitor molecules can absorb on aluminum surface on the basis of
donor-acceptor interactions between π-electrons of aromatic rings and vacant p-orbitals of surface aluminum atoms.
Thus, we can conclude that inhibition of aluminum corrosion in HCl is mainly due to electrostatic interaction. The

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decrease in inhibition efficiency with rise in temperature (Table 7) supports electrostatic interaction. The order of
decreasing inhibition efficiency of the compounds from all techniques used is: inhibitor 2 ˃ inhibitor 1. Inhibitor 2 has
the highest percentage inhibition efficiency, this being due to its larger molecular size than compound (1) which cover
larger area from aluminum surface. Also, NO2 group in compound (2) may reduce in HCl and the secondary product is
the compound which adsorbed on aluminum surface.

IV.CONCLUSIONS
The investigated compounds are good inhibitors for the corrosion of aluminum in HCl solutions and they act as mixed
type inhibitors. The results obtained from all the electrochemical measurements show that the inhibition properties
increase with small differences in their %IE numerical values. Double layer capacitances decrease with respect to blank
solution when these compounds were added. This fact may explained by adsorption of these molecules on the
aluminum surface. The adsorption of the investigated chalcone derivatives on aluminum surface in HCl solution
follows Langmuir adsorption isotherm. The negative values of ΔG°ads show the spontaneity of the adsorption process.

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