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JMEPEG (2015) 24:839847

DOI: 10.1007/s11665-014-1325-9

Effect of Silica Ratio on the Corrosion Behavior

of Nano-silica Potassium Silicate Coatings
on Aluminum Alloy 2024
H. Bahri, I. Danaee, G.R. Rashed, and D. Zaarei
(Submitted December 19, 2013; in revised form August 17, 2014; published online December 2, 2014)
Nano-silica modied potassium silicate conversion coating was deposited in different nano-silica/potassium
silicate ratios on the surface of 2024 aluminum alloy. The corrosion behavior of coatings was studied by
electrochemical impedance spectroscopy, current transient, potentiodynamic polarization, and surface
techniques. The ratio of nano-silica/potassium silicate was optimized in order to obtain higher corrosion
protection. The experimental results indicated that with increasing nano-silica/potassium silicate ratio, the
corrosion resistance of aluminum increases. Furthermore, the pitting corrosion probability of potassium
silicate conversion coating decreased with increasing silica ratio. This can be related to the size of nanosilica particles and the ability to ll the pores in potassium silicate coating and reinforce the created siloxane
bridges.

Keywords

aluminum 2024, corrosion, nano-silica, silicate conversion coatings

1. Introduction
Aluminum and its alloy is one of the materials, which has an
important role in the engineering structures and its usage
ranking stands only behind the ferrous alloys. Some special
properties of this metal include: its strength, density ratio,
toughness, and corrosion resistance (Ref 1). To attain appropriate attributes, aluminum can be alloyed with different metals,
such as: magnesium, silicon, copper, zinc, iron, manganese,
lithium (Ref 2-4). Aluminum alloy AA2024 is used greatly in
aerospace industries because of its excellent mechanical
properties and low density (Ref 5, 6). Materials such as copper,
magnesium, zinc, and iron in this alloy decrease the corrosion
resistance signicantly due to the formation of the intermetallic
compounds (IMCs) (Ref 7-11). Pure aluminum has a good
corrosion resistance due to the formation of a strong oxide
layer, but AA2024 involves IMCs which form small galvanic
cells in aluminum matrix and lead to localized corrosion
(Ref 12-15). One way to increase the corrosion resistance and
protect these alloys is coatings. Conversion coatings are an
important group of these coatings which usually have a thin
thickness, provide corrosion protection and enhance the
adhesion between different coating layers (Ref 16, 17). Chromate conversion coatings (CCCs) are the most common and
effective anti-corrosive treatments for aluminum alloys

H. Bahri, I. Danaee, and G.R. Rashed, Abadan Faculty of Petroleum

Engineering, Petroleum University of Technology, Abadan, Iran; and
D. Zaarei, Technical Faculty, South Tehran Branch, Islamic Azad
University, Tehran, Iran. Contact e-mail: danaee@put.ac.ir.

Journal of Materials Engineering and Performance

(Ref 17-19). Although CCCs provide a great corrosion resistance, they are toxic and carcinogenic due to the presence of
hexavalent chromium; therefore, these coatings are under strict
regulations (Ref 20, 21). Due to the toxicity of Cr6+, several
studies have been done on the replacements for CCCs and the
extension of non-toxic coatings (Ref 22). Silicate conversion
coatings are one of the best superior alternatives for the CCCs
(Ref 23, 24). These coatings have a good durability against
each kind of corrosion and are safe for the humans and
environment (Ref 23, 25, 26). Many studies showed that the
silicate coatings provide good corrosion resistance for the
substrate metals (Ref 27-31). Alkali silicates are common and
general group of silicate coatings. Alkali silicate solutions
contain two fractions: (a) alkali ions, hydroxide ions, and
silicate ions (SiO44), (b) polymerized (colloidal) fractions. The
very large polymerized particles are a complex mixture of
polysilicate anions and their hydroxylated surfaces which
consist of silanol (-Si-OH) groups and siloxane bridges (-Si-OSi-). During the drying process, polymerization continues and
more silanol groups are converted to the siloxane bridges. The
produced layer on the substrate increases the corrosion
resistance (Ref 32-34). However, pristine silicate conversion
coatings are still permeable to corrosive agents such as water,
oxygen, and destructive ions like Cl, H+, SO42. This is due
to the porous structure of conversion coatings which lead to
increasing the susceptibility to pitting corrosion. In order to
enhance the barrier properties of these conversion coatings,
various methods and additives have been used by a great
number of researchers (Ref 23, 25, 28, 34). Min et al. (Ref 23)
studied the effect of potassium methyl siliconate on the anticorrosion properties of the silicate conversion coating on
galvanized steel. They veried that the addition of potassium
methyl siliconate into silicate coatings increased the corrosion
protection ability of coatings due to the formation of the more
hydrophobic surface. The substantial concentration of K ion at
the coating surface was decreased by the addition of potassium
methyl siliconate which decreased the hydrophobic properties.

Volume 24(2) February 2015839

In the present study, potassium silicate conversion coating

modied with nano-silica was applied on AA2024 in different
nano-silica weight ratio. Addition of nano-silica increases the
stability and continuity of silicate conversion coatings due to
the size of nanoparticles and their ability to ll the porous
properties of these coatings. The effect of nano-silica on the
anti-corrosion properties of the silicate conversion coatings
were investigated by means of electrochemical impedance
spectroscopy (EIS) and polarization curves in 3.5 wt.% NaCl
solutions. Surface morphology, chemical composition, and
microscopic features of conversion coating were analyzed by
scanning electron microscopy (SEM) and energy-dispersive
spectroscopy (EDS).

105-102 Hz with AC signal amplitude of 10 mV. Fitting of

experimental impedance spectroscopy data to the proposed
equivalent circuit was done by means of a home written least
square software based on the Marquardt method for the
optimization of functions and Macdonald weighting for the real
and imaginary parts of the impedance (Ref 35, 36).
The morphology of the surface was studied by metallographic microscope (Neophot 32) and SEM (VEGA, TESCANLMU) equipped with an energy-dispersive x-ray spectroscopy
(EDS) probe. Salt spray tests were carried out in CTS-114D salt
spray fog chamber (B.AZMA).

3. Results and Discussion

2. Materials and Methods

3.1 Effect of Potassium Silicate Concentration

2.1 Materials
Aluminum alloy 2024 was purchased and the major alloying
elements are: Cu: 3.8-4.6, Mg: 1.3-1.6, Mn: 0.5-0.8, Si: < 0.5,
Fe: < 0.5, Zn: < 0.25, Ti: < 0.15, Cr: < 0.1, V: < 0.05, Zr:
< 0.05, others: < 0.15%wt and Al: Rest. Samples were
subjected to mechanical polishing with sand papers of 400 to
2000 grades, and cleaned with acetone. To remove any trace of
surface oxides, the samples were immersed in NaOH for 30 s
and then immersed in dilute H2SO4 solution for 30 s. Between
each step, the panels were rinsed with deionized water.
A 40 wt.% aqueous solution of potassium silicate with
silicate/alkali molar ratio of 2 was prepared from the Iran Silis
Company. A 30 wt.% aqueous solution of colloid nano-silica
with 20-30 nm particle size was prepared from Iranian
Nanomaterials Pioneers. Different concentrations of potassium
silicate solution and nano-silica colloidal solution were mixed
and different silica ratios, 2:11, 2:16, 2:22, 2:33, and 2:44, were
provided. Silicate conversion coatings were obtained by dip
immersion method. Aluminum samples were immersed for
400 s in prepared water-based coating solution in different
silica ratios, and the coated samples were cured in oven at
150 C for 30 min. The coated samples were stored at room
temperature for 1 h.

Figure 1 shows the potentiodynamic polarization curves of

aluminum2024 with and without silicate coatings in 3.5%wt.
NaCl solution. Silicate coatings were obtained from different
concentrations of potassium silicate solution. The corresponding corrosion parameters such as corrosion current density
(Icorr), corrosion potential (Ecorr), anodic slope (ba), cathodic
slope (bc), polarization resistance (Rp), and corrosion rate (CR)
are listed in Table 1. The polarization resistance is calculated by
the following equation (Ref 37):

2.2 Electrochemical and Surface Morphology Investigation

Electrochemical measurements were carried out by Potentiostat/Galvanostat Autolab, model PGSTAT 302 N. Electrochemical glass cell contained a reference electrode of Ag/AgCl,
an auxiliary electrode of platinum and a sample of coated 2024
aluminum alloy as the working electrode. To provide steady
state condition, the samples were stored for 30 min in
electrolyte solution before the test. The scan rate of polarization
curves was 1 mV/s. The frequency range of the EIS was

Fig. 1 Polarization curves of silicate coated aluminum 2024 in

3.5 wt.% NaCl solution. Silicate coating was obtained from different
potassium silicate concentrations with ratio 2: (1) bare sample, (2) 1,
(3) 2, and (4) 3 M

Table 1 Electrochemical parameters of the silicate coatings in 3.5 wt.% NaCl solution
Samples

Ecorr, V

Icorr, A/cm2

ba, V/dec

bc, V/dec

R p, X

Vcorr, mm/y

Bare
1M
2M
3M

0.668
0.609
0.572
0.617

8.47 9 107
4.19 9 107
1.45 9 108
4.11 9 109

0.005
0.095
0.03
0.17

0.012
0.113
0.144
0.151

1.82 9 103
5.34 9 104
7.39 9 105
8.46 9 106

4.14 9 103
4.92 9 103
1.71 9 104
4.16 9 105

Coatings were obtained from different concentrations of potassium silicate solution in ratio 2

840Volume 24(2) February 2015

Journal of Materials Engineering and Performance

Fig. 2 SEM images of silicate coated AA2024 sample after polarization test. Silicate conversion coating was obtained from (a) 1 M and
(b) 3 M potassium silicate solution. Some pits are shown in this gure

Rp

ba bc
1

:
2:303ba bc Icorr

As can be seen, the corrosion current densities decrease in

the presence of the silicate coatings. During the curing step,
trapped water in the conversion coating evaporated and silicate
networks (siloxane bridges) created. Corrosion protection was
mainly due to the formation of silica rich Al-oxide lm. Silicate
formed a protective layer and incorporated in the pores of Aloxide lm to form a high corrosion-resistant layer. Both the
anodic and cathodic branches of the polarization curves for
silicate coating shift to lower corrosion current densities
indicates that both the anodic and cathodic reaction blocked.
Potentiodynamic scans and their corresponding parameters
show that the increase of potassium silicate concentration in the
coating bath leads to increasing in the coating resistance. This

Fig. 3 Polarization curves of the silicate coatings in 3.5 wt.% NaCl

solution. Coatings were obtained from different concentrations of
potassium silicate solution with ratio 2:16 (1) bare AA2024, (2) 0:5,
(3) 1, (4) 2, and (5) 3 M

Journal of Materials Engineering and Performance

phenomenon was due to the reinforcement and the completion

of the siloxane bridges.
The silicate coating, prepared from 1 M potassium silicate
solution, showed pitting corrosion (Fig. 1). The current density
in the anodic branches of this coating increases due to the pit
nucleation. Moreover, according to Fig. 1, pitting corrosion of
all silicate coatings is lower than the bare aluminum which is
susceptible to pitting corrosion in NaCl solution (Ref 38, 39).
Figure 2 shows the SEM image of silicate coated electrode
surface obtained from 1 and 3 M potassium silicate solution
after the polarization test. As can be seen, the surface of the
silicate coated sample, obtained from 1 M potassium silicate,
depicts the discontinuities and some pits (Fig. 2a). It can be
related to the defects and imperfections of the silicate networks
which led to the permeation of the chloride ions and
deterioration of the protective layer. By means of increment
in silicate concentration, no increase of current was observed in
the anodic branches of these coatings. This was due to the
relative completion in silicate surface and the decrease of the
surface pores. In addition, according to Fig. 2b, the imperfections and damages of pitting corrosion in the silicate networks
decrease after polarization.
Figure 3 shows the effect of increasing the ratio by nanosilica for different concentrations of potassium silicate on the
corrosion resistance of conversion coating. The corresponding
electrochemical parameters of polarization curves are presented
in Table 2. The corrosion current density and the corrosion rate
decrease, and the polarization resistance increases in the
presence of nano-silica. The size of the nano-silica particles
was the most important effect which lled the pores and spaces
of the silicate networks (Ref 34) and improved the uniformity
of the silicate layers (Ref 40). The high surface area was
another benet of these particles which provided higher
contacts between functional groups and more convenience
condition to create silicate networks (Ref 41). Furthermore,
Padavettan (Ref 41) believes that nano-silica particles can
decrease the sintering temperature of silicate coatings and
produce stronger siloxane bridges at the same preparation
conditions. Therefore, the presence of nanoparticles improved
the corrosion characteristic of protective layer. As shown in the
Fig. 3 and Table 2, the best corrosion resistance was achieved

Volume 24(2) February 2015841

Table 2 Electrochemical parameters of the silicate coatings in 3.5 wt.% NaCl solution
Samples

Ecorr, V

Icorr, A/cm2

ba, V/dec

bc, V/dec

R p, X

Vcorr, mm/y

0.5 M
1M
2M
3M

0.985
1.083
1.142
1.225

6.09 9 109
9.93 9 1010
3.17 9 109
8.98 9 109

0.138
0.096
0.252
0.209

0.087
0.212
0.285
0.257

3.80 9 106
3.07 9 107
1.82 9 107
5.57 9 106

3.76 9 105
2.46 9 105
3.22 9 105
5.05 9 105

Coatings were obtained from different concentrations of potassium silicate solution in ratio 2.16

Table 3 Electrochemical parameters of the silicate coatings in 3.5 wt.% NaCl solution
Samples

Ecorr, V

Icorr, A/cm2

ba, V/dec

bc, V/dec

R p, X

Vcorr, mm/y

Ratio
Ratio
Ratio
Ratio
Ratio

0.609
1.079
1.132
1.082
1.235

4.19 9 107
3.88 9 109
8.93 9 1010
1.26 9 1010
1.74 9 109

0.095
0.114
0.115
0.066
0.04

0.113
0.265
0.347
0.085
0.259

5.34 9 104
8.91 9 106
4.19 9 107
1.28 9 108
0.96 9 107

4.92 9 103
4.56 9 105
1.17 9 105
1.48 9 106
2.04 9 105

2
2:11
2:22
2:33
2:44

Coatings were obtained from 1 M potassium silicate solution in different ratios

at 1 M potassium silicate. The regular and appropriate porous

silicate layers were created at this concentration. The nanoparticles had suitable freedom to ll the pores and complete the
silicate networks. But at higher concentrations, the porous
properties of the silicate coatings decreased (Ref 25, 34, 42).

3.2 Effect of Nano-silica Ratio of Potassium Silicate

Figure 4 presents the effect of increasing the Si/K ratio of
potassium silicate on the corrosion resistance of conversion
coatings. The corresponding corrosion parameters are presented
in Table 3. The ratio was increased for 1 M potassium silicate
by nano-silica addition. With increasing silica ratio up to 2.33,
the corrosion resistance of the silicate layer increases and the
corrosion rate and the pitting corrosion probability decrease. In
addition, both the anodic and cathodic branches of the
polarization curves move toward the lower current densities.

Fig. 4 Polarization curves of the silicate coatings in 3.5 wt.% NaCl

solution. Coatings were obtained from 1 M potassium silicate solution in different ratios: (1) bare AA2024, (2) ratio 2, (3) ratio 2:11,
(4) ratio 2:22, (5) ratio 2:33, and (6) ratio 2:44

842Volume 24(2) February 2015

No pitting initiation is observed in this potential range of the

anodic branches (Ref 43). Silicates with higher number of
nanoparticles had the more polymeric units for the formation of
siloxane bridges during the curing process. Moreover, silicate
surfaces are water absorbent due to the positive charge of
surface, namely potassium. Colloidal silica has a negative
charge and can bind to the positive charges. Therefore, in the
presence of nano-silica, hydrophilic sites decreased and the
hydrophobic property of silicate layers increased which provided greater corrosion protection. In the higher silica ratios,
the corrosion rate increase due to the internal stress which
decreased its toughness and led to increasing the cracks. During
the curing step in oven, a few cracks created on the surface due
to the drying process and therefore, the corrosion resistance of
the coatings decreased.
Figure 5 shows the current transient of AA2024 at 0.3 V
versus Ag/AgCl in different ratios. At the beginning, the
current decreases as a function of time which indicated the
formation of some protective oxide layer and the double-layer
charging. In the absence of nano-silica (Fig. 5a), the current
increases drastically until reaches to a maximum quantity. This
increasing current showed the nucleation and development of
the pits. In the longer times, the repassivation of the pits
occurred which led to decreasing current. Finally the current
reaches to a steady state value which is higher than its initial
value due to the pitting corrosion (Ref 44, 45). In the higher
silica ratio with nano-silica, no increasing current was observed
and the pitting corrosion resistance of the silicate conversion
coatings increases (Fig. 5b).
Electrochemical impedance was employed to conrm the
anti-corrosion behavior of the silicate coating. Figure 6 shows
the Nyquist plots of silicate coated aluminum obtained in
different ratios of silica. Impedance was measured at open
circuit potential in 3.5%wt. NaCl solution. The data reveal that
the impedance diagrams consist of a depressed capacitive loop
which is due to the charge transfer resistance and double-layer
capacitance. The equivalent circuit compatible with the Nyquist
diagram is depicted in Fig. 7. In this electrical equivalent
circuit, Rs, Qdl, and Rct represents solution resistance, a constant

Journal of Materials Engineering and Performance

Fig. 5 Current transient diagrams of potassium silicate coatings in

3.5 wt.% NaCl solution. (a) Coatings were obtained from 1 M potassium silicate solution in ratio 2. (b) Coatings were obtained from
1 M potassium silicate solution in different ratios: (1) 2:16 and (2)
2:33

phase element corresponding to the double-layer capacitance

and the charge transfer resistance, respectively. To obtain a
satisfactory impedance simulation of silicate coated aluminum,
it was necessary to replace the capacitor (C) with a constant
phase element (CPE) Q in the equivalent circuit. The most
widely accepted explanation for the presence of CPE behavior
and depressed semicircles on solid electrodes is microscopic
roughness, causing an inhomogeneous distribution in the
solution resistance as well as in the double-layer capacitance
(Ref 46, 47).
To corroborate the equivalent circuit, the experimental data
were tted to equivalent circuit and the circuit elements were
obtained. Table 4 illustrates the equivalent circuit parameters
for the impedance spectra of silicate coated aluminum in NaCl
solution. From Table 4, with increasing silica ratio, the coating
resistance increases. This was due to the presence of the more
uniform silicate coating on the surface of AA2024, which
decreased the active area of the substrate.
Figure 8 shows the SEM images and the corresponding
EDS spectrum of potassium silicate coatings obtained from
1 M solution without nanoparticles. The EDS results represent
the weight percentages of the coating elements. The potassium

Journal of Materials Engineering and Performance

Fig. 6 Electrochemical impedance spectroscopy diagrams of potassium silicate coatings in 3.5 wt.% NaCl solution. (a) Coatings were
obtained from 1 M potassium silicate solution and ratio 2. (b) Coatings were obtained from 1 M potassium silicate solution in different
ratios: (1) 2:11, (2) 2:22, and (3) 2:33

Fig. 7 Equivalent circuit compatible with the Nyquist diagram of

potassium silicate conversion coatings of AA2024

silicate conversion coatings contain the discontinuities and

agglomerates which related to the silicate networks and the
defects of these layers. The coating defects are the susceptible
zones for the corrosion attacks. Figures 9 and 10 show the
surface of the silicate conversion coatings with higher ratio of
silica. Both coating surfaces are homogeneous without discontinuities and irregularities on surfaces. The brighter zones on
the surface with nano-silica can be related to the nano-silica
particles that remained unchanged on the surface and did not
participate in the polymerization. These brighter zones cannot

Volume 24(2) February 2015843

Table 4 EIS parameters of the silicate coatings in 3.5 wt.% NaCl solution
Sample
Ratio
Ratio
Ratio
Ratio

2
2:11
2:22
2:33

Rs, X

Rct, X

Qdl, F

17
18
18
16

9.2 9 105
3.2 9 107
5.3 9 107
1.4 9 108

7 9 105
3 9 107
2 9 108
4 9 108

0.80
0.75
0.83
0.83

Coatings were obtained from 1 M potassium silicate solution in different ratios

Fig. 8 (a) SEM and (b) EDX analysis of the potassium silicate
conversion coating obtained from 1 M potassium silicate with ratio 2

be seen in Fig. 8. The results of EDS analysis are shown in

Table 5. The results indicated that the Si:K weight ratio
increases in the presence of nano-silica. The ratio of potassium
silicate without nano-silica is 1:58. In presence of nanoparticles, the silica ratios were increased to 2:03 and 2:32. Figure 11
shows the SEM image of the nano-silica conversion coating
obtained from ratio 2:44. It was found that the cracks increased

844Volume 24(2) February 2015

Fig. 9 (a) SEM and (b) EDX analysis of the potassium silicate
conversion coating obtained from 1 M potassium silicate with ratio
2.16

and progressed during the drying process which was in

agreement with the polarization data. Cracks created during
the drying process for all ratios of silicate conversion coatings.
Figure 12 shows the SEM images of nano-silica potassium
silicate conversion coatings after polarization test. Silicate

Journal of Materials Engineering and Performance

Fig. 11 SEM image of the potassium silicate conversion coating

obtained from 1 M potassium silicate with ratio 2.44

Table 5 EDS results of the 1 M potassium silicate

surface coatings in different ratios of silica
Ratio
Ratio 2
Ratio 2:16
Ratio 2:33

Weight% of Si

Weight% of K

Weight% of O

29.76
33.85
30.58

18.75
16.67
13.15

51.49
49.48
56.27

Fig. 10 (a) SEM and (b) EDX analysis of the potassium silicate
conversion coating obtained from 1 M potassium silicate with ratio
2:33

coating was prepared from 1 M silicate solution with silica ratio

2:33. According to this image, surface corrosion of silicate
coating is negligible and no pits and discontinuities are
observed on the coating. This was due to the effects of
nanoparticles on the stability and the corrosion resistance of the
silicate coatings.
The salt spray test (SST) was performed in accordance with
ASTM B117 (Ref 48) with an exposure time of 8 days.
Figure 13 shows the optical surface image of the silicate
conversion coatings of aluminum 2024 after the salt spray test.
Conversion coatings were obtained from 1 M potassium
silicate solution in different ratios of SiO2/K2O. In the absence
of nano-silica, aluminum is corroded and some pits create on its
surface (Fig. 13a). On the other hand, with increasing the silica
ratio, a glassy and uniform coating remained after corrosion test
(Fig. 13b). In addition, no pits and corroded area were
observed. These data conrmed the positive effect of nano-

Journal of Materials Engineering and Performance

Fig. 12 SEM image of the potassium silicate conversion coating

after polarization rest. Silicate conversion coating was obtained from
1 M potassium silicate with ratio 2:33

Volume 24(2) February 2015845

Fig. 13 Visual aspect of 60 9 55 mm silicate coated samples after 8 days of exposure to SST. Coatings were obtained from 1 M potassium silicate solution in different silica ratios: (a) 2 and (b) 2:33

silica on the corrosion resistance of the silicate coatings. This

enhanced corrosion resistance was originated from the
increased in the hydrophobicity of the coating layer.

4. Conclusion
The corrosion behavior of nano-silica potassium silicate
conversion coatings on the 2024 aluminum alloy was investigated in 3.5 wt.% NaCl solution. Potassium silicate coatings
improved the corrosion resistance of the aluminum due to the
formation of silicate lm. But this protective barrier had some
discontinuities and defects which led to decreasing its stability
and increasing the pitting corrosion probability. Presence of
nano-silica improved the silicate networks and decreased the
existing defects. The ratio of nano-silica played an important
role to provide a high corrosion protection. Silicate conversion
coatings from 1 M potassium silicate solution with silica ratio
2:33 was more protective and continuous. The high corrosion
resistance was mainly due to the formation of compact and
perfect silicate layers on the surface in the presence of nanosilica.

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