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Corrosion Characteristics of Zn-TiO2 Nanocomposite Coatings Fabricated by

Electro-Codeposition Process

Article · January 2024

DOI: 10.48309/ajca.2024.418391.1425

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 Advanced Journal of Chemistry, Section A, 2024, 7(2), 209-226

Advanced Journal of Chemistry, Section A

journal homepage: www.ajchem-a.com

Original Research Article

Corrosion Characteristics of Zn-TiO2 Nanocomposite Coatings

Fabricated by Electro-Codeposition Process
Mohammad Sajjadnejad1* , Sara Karkon1, Seyyed Mohammad Saleh Haghshenas2
1Department of Materials Engineering, School of Engineering, Yasouj University, Yasouj, Iran
2Department of Materials Science and Engineering, School of Engineering, Shiraz University, Shiraz, Iran

ARTICLEINFO ABSTRACT
Article history Zn based composite coatings reinforced with TiO2 nanoparticles were
fabricated via electrodeposition with 5, 10, and 15 g/L TiO2 concentration
Submitted: 15 October 2023
under variant current densities of 0.08, 0.1 and 0.12 A/cm2. Field emission
Revised: 19 November 2023 scanning electron microscopy (FESEM), energy dispersive spectroscopy
Accepted: 01 December 2023 (EDS), x-ray diffraction analysis (XRD), weight loss measurements, salt spray
Available online: 10 December 2023 technique, anodic polarization, and eventually potentiodynamic polarization
tests were conducted and the corresponding findings were discussed. Rising
Manuscript ID: AJCA-2309-1425 the electrodeposition current density from 0.08 to 0.12 A/cm2 for both pure
Checked for Plagiarism: Yes Zn and Zn-TiO2 coatings led to deposit more and smaller crystals and with
Language editor: incorporation of TiO2 nanoparticles, the morphology changed from hexagonal
Dr. Fatimah Ramezani crystals to flake type grains. Increasing the TiO2 concentration from 5 to 15
Editor who approved publication: g/L, steadily lowered the TiO2 incorporate rate (vol.%). Accordingly, the same
smoothness and even more uniformity with smaller crystallites was observed
Dr. Umer Rashid
at 15 g/L compared to that of 5 g/L. Weight loss measurements, salt spray
DOI: 10.48309/ajca.2024.418391.1425 tests and anodic polarization test showed remarkable superior corrosion
resistance of Zn-TiO2 (5 g/L) than that of pure Zn coating. An increas in icorr
KEYWORDS (µA/cm2) from 0.08 to 0.1 A/cm2 occurred, followed by a decrease from 0.1 to
Electro-codeposition 0.12 A/cm2 for pure zinc coating. By increasing the current density from 0.08
Nanocomposite coating to 0.12 A/cm2 for Zn-TiO2 coating, a steadily decrease of icorr was observed.
Zinc Furthermore, by rise of TiO2 (%C) from 5 to 15 g/L, icorr experienced a
TiO2 significance increase that could be ascribed to the remarkable reduction in
Corrosion characteristics TiO2 vol.%. Ultimately, the optimum corrosion resistance belonged to the
Morphology electrodeposited Zn-TiO2 (5 g/L) coating deposited 0.12 A/cm2 exhibiting the
lowest amount of icorr of 2.7 µA/cm2 equal to 1.6 mpy.

* Corresponding author: Dr. Mohammad Sajjadnejad

 E-mail: [email protected]; [email protected]
© 2024 by SPC (Sami Publishing Company)
 M. Sajjadnejad et al. / Adv. J. Chem. A 2024, 7(2), 209-226

GRAPHICALABSTRACT

Introduction coatings concerns arise due to the formation of

white rust. To be more specific, white rust
In recent decades, zinc has been widely applied formation can be mitigated for a limited time
as a well-known coating on the steel surface to while the deposition of chromate conversion
enhance its corrosion resistance. The application coating occurs. Although, this process has been
of zinc coating on steel surface is performed recently kept away from application due to
through electrolysis or galvanization. Given that environmental hazards [3]. Today, eco-friendly
zinc is a metal with higher activity (more materials have attained increasingly attention
negative electrochemical potential) compared to and investigation on the metal matrix composite
steel, thus zinc must be protected to increase the coatings has been going on for a long time. In
service life of coating as well as steel [1]. Due to recent years, targeted environmental plans have
high corrosion rate of zinc coating in very strong led to remove chromium based coatings and
and aggressive acidic or alkaline environments, fabricated new eco-friendly composite coatings
they are normally used in the pH range of 6-12. with the assistance of nanotechnology resulting
Moreover, zinc coatings are too fragile to be in new developments in nanocomposite coatings
applied in harsh corrosive environments like [4,5].
those containing pollutants produced in various Applying corrosion inhibitors is regarded as
industries [2]. Remarkable properties of another strategy to increase the service life of the
employing chromate conversion coating on zinc zinc coated materials to modify their surface
evoked interest among researchers in recent behavior [6]. Most of the inhibitors are organic
years [1]. Having said that, chromate coatings are compounds containing nitrogen, sulfur and/or
unstable at temperatures higher than 70 C. oxygen elements. Compounds with functional
Moreover, during the production of chromate, groups containing hetero-atoms, highly promote
the corrosion inhibition. In general, these

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compounds are adsorbed on metal surface and fabricate metal matrix composite coatings, it can
block the active sites of corrosion [7] and provide be chosen as the best alternative for production
a barrier between corrosion medium and metal. of metal matrix composite (MMC) coatings [18-
As a result, the interaction between metal atom 24].
and environment will be reduced and the The composite coatings are of high significance
formation of white rust will be also controlled. in recent years, owing to the successful
However, the chromium ions and organic incorporation of nanoparticles in the process of
inhibitors are liberated to the environment as the co-deposition by electrolysis. This technique is
corrosion occurs. These compounds are toxic in carried out under a normal pressure and room
nature and produces pollution and serious health temperature, and often possesses a high level of
hazards. What is more, in severe corrosive deposition rate. Electrodeposition has been well
medium, the protective layer gets damaged as known as one of the most important approaches
the result of severe corrosion. One of the most in order to fabricate nanocrystals and above all
important difficulties, here, is the method for nanocomposites, where nano-sized particles
application of chrome passivation due to such as SiC, TiO2, Al2O3 [25], ZnO [26], WC, PTFE,
requiring expert skills [8]. SiO2, CNTs, CeO2 [27], Ni3S4 [28], MoS2 [29],
Thus, one of the most increasingly interested graphene [14], diamond [30], etc. have been
solution to modify zinc coating and other metal- evoked scientific importance in metal matrix
based coating properties is to introduce second composite coatings (particularly in zinc coating),
phase reinforced particles into the base metal due to their magnificent role on the hardness
matrix and create a composite coating. improvement, self-lubrication, wear and
Fabrication of composite coatings has been corrosion resistance, and also compatibility in
widely employed as a highly useful approach biological and chemical fields [4,15,19,23,31-36].
where ceramic, oxide, and also polymeric micro- More importantly, electrodeposited coatings
particles or nano-particles are co-deposited on possess unique characteristics namely, high
the metal surface using suitable electrolyte. corrosion resistance, self-lubricity, high
These composites have a wide range of temperature inertness, and biological
properties such as dispersion hardening, self- compatibility [31,37]. TiO2 possesses also various
lubricity, high temperature inertness, good wear useful applications in different kinds of industrial
and corrosion resistance, and chemical and and domestic fields such as metallic and organic
biological compatibility [5, 9-17]. coatings, catalysis applications as catalyst
Among the major fabrication techniques to support, wastewater treatment, and photovoltaic
produce metal composite matrix, liquid and cells. The photocatalytic activity of TiO2 has
solid-state methods cannot be able to attracted highly attention in various metallic and
manufacture thin films. Furthermore, spray organic coatings [38-44], and also in Zn plating
forming or spray deposition technique, and also on steel has been reported [45,46]. Another
chemical vapor deposition (CVD) processes can important advantage of TiO2 comes from its high
be only performed at high temperatures which is ability in reinforcing metallic coatings to greatly
a major disadvantage of these methods. enhance the corrosion and wear resistance,
Thus, electroless plating and electrodeposition hardness, and other mechanical characteristics,
can only be applied for fabrication of metal and also magnetic properties [47]. There are
matrix composite (MMC) at ambient several research works that made a thorough
temperatures. Since the electrodeposition investigation on the electrodeposition and
technique has been utilized to a large extent to corrosion characteristics of Zn-TiO2 composite

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coating [48-51]. However, these studies are nanoparticles, (5) ions cloud, (6) anode, (7) cathode,
limited and there is a need of a comprehensive (8) magnetic stirrer, and (9) reference electrode.
study on the electrodeposition and TiO2 nanopowder was purchased from US
microstructure-corrosion resistance relationship. Research Nanomaterials and possess anatase
The main purpose of this research study is to phase. The specifications of TiO2 nanopowder are
explore and assess the electrodeposition of Zn- reported in Table 1.
TiO2 nanocomposites and their corrosion Moreover, SEM micrograph, TEM image, and
behavior upon the obtained results from weight XRD patterns of the aforementioned nano TiO2
loss, salt spray, electrochemical methods (anodic powders are depicted in Figures 2 to 4,
polarization and potentiodynamic polarization), respectively.
and surface morphology after corrosion process.
The relation between surface morphology of
electrodeposited coatings, XRD measurements,
and corrosion properties were also determined.

Materials and methods

In this study, the pure zinc and Zn-TiO2

nanocomposite coatings specimens were
electrolytically deposited in a sulphate bath. The
constituents of the bath were 200 g/L ZnSO4, 20
g/L H3BO3 (for keeping pH constant), 0.3 g/L
sodium dodecyle sulfate (SDS), and certain Figure 2. SEM micrograph of TiO2 nano powders.
content of titanium dioxide (TiO2) nanoparticles
possessing a particle size ranging from 40 to 50
nm. Figure 1 displays a schematic presenting the
experimental setup utilized for electrodeposition
of pure zinc and zinc-nano TiO2 composite
coatings.

Figure 3. TEM image of TiO2 nano powders

Figure 1. Experimental setup of electrodeposition, (1)

pulse power supply, (2) plating solution, (3) TiO2
nanoparticles in composite, (4) suspended TiO2

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according to its sacrificial behavior. The low

carbon steel was mechanically polished and
degreased with acetone followed by water wash.
Dipping in 10% HCl was employed to activate the
zinc surface for few seconds, then was water-
washed.
The area of anode was 3 times higher than
cathode for prevention of anodic polarization.
The bath temperature was at room temperature
(298 K) and pH of the bath was set at 4.5. The
electrodeposition process was carried out under
Figure 4. XRD pattern of TiO2 nanoparticles. mechanical stirring. Bath composition is
indicated in Table 2.
Analytical reagents and distilled water were After the electroplating process, specimens were
utilized to prepare the plating solution. Before studied by X-ray diffraction (XRD) analysis via a
plating occurs, the TiO2 nanoparticles with a Philips X-pert-pro diffractometer with a copper
mean diameter of 40-50 nm were dispersed in Kα source. The weight loss measurements were
the electrolyte. The nanoparticles were easily performed for low carbon steel specimens which
agglomerated owing to their high surface energy, were coated with pure zinc and Zn-TiO2
followed by controlling the agglomeration owing nanocomposites. To assess the corrosion
to the addition of a surfactant like SDS to the behavior of nanocomposite coatings, an equal
bath. The bath was stirred for 24 hours before area of specimens was immersed in NaCl solution
conducting electrocodeposition experiments. (3.5 wt.%) at room temperature. The loss in
Low carbon steel was chosen as the cathode and weight was measured once in every 72 hours for
anode was zinc (99.96%) which could a period of 9 days.
compensate the consumption of zinc ions
Table 1. Specifications of nano TiO2 powders
Variable Range
Type of nanoparticles Anatase phase
Particle size 40-50 nm
Surface area > 150 m2/g
Purity percentage + 99
Appearance White powder
Density 4.23 g/cm3

Table 2. The solution composition and electrodeposition parameters

Variable Range
ZnSO4.7H2O 200 g/l
H3BO3 20 g/l
SDS 0.3 g/l
TiO2 nanoparticles 0, 5, 10, 15 g/l
Temperature 25 ℃
Current density 0.8, 0.10, 0.12 A/cm2
pH 4.5
Stirring rate 250 rpm

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After the experiment, the corroded samples Results and Discussion

were rinsed in H2SO4 15 wt.% solution, dried in
hot air, and then the weight loss was noted. The SEM and EDS Analyses
weight loss measured was applied on calculation
As it is displayed in Figure 1, the FESEM images
the corrosion rate. Salt spray test (according to
of deposited zinc coatings are observed in
ASTM B117) was also performed in order to
different current densities (0.08, 0.1 and 0.12
make a comparison between the corrosion
A/cm2).
characteristics of pure zinc and Zn-TiO2
As it is observed in Figure 5, zinc deposits have
nanocomposite coatings. Specimens were
a hexagonal platelet microstructure [52,53].
subjected to continuous neutral spray of 5% NaCl
According to Figure 5a, one hexagonal crystal of
vapors. The specimens were investigated
zinc is observed, while the number of these
carefully and the period for formation of the
crystals is increased by increasing the current
white rust on coatings was noted. A conventional
density. To be more specific, applied current acts
3-electrode cell was used for potentiodynamic
as the main driving force for ion mobility to
polarization studies. The pure zinc-coated and
cathode surface leading to a higher reduction
Zn-TiO2 nanocomposite coated specimen were
rate of ions and subsequently smaller and more
employed as working electrode with active
crystals [52-55]. Figure 6 also shows FE-SEM
surface area of 3 cm2. Saturated calomel
images of zinc composite coatings are observed
electrode (SCE) and graphite were used as
in different current densities.
reference and counter electrodes, respectively.
Clearly, by incorporation of TiO2 nanoparticles
The potentiodynamic polarization measurements
into the zinc matrix, remarkable grain refinement
and also anodic polarization curves were drawn
occurs and the general morphology of zinc
to assess the corrosion resistance of coating
converts drastically from a hexagonal platelet
samples. The electrolyte was 3.5 wt.% NaCl
state to flake type grains. This proves that
solution for anodic polarization tests and 1M
increasing the nucleation sites and also grain
NaCl for potentiodynamic polarization tests.
boundaries cannot be sustained by hexagonal
Potentiodynamic polarization tests were carried
platelet microstructure in zinc metal and results
out via computer controlled the Autolab PGSTAT
into formation of a highly different morphology
302N equipment by the scan rate of 1 mV/s.
of zinc-matrix composites. This kind of grain
The morphology of the deposited specimens
refinement and reduction in crystal growth is
was studied before and after corrosion tests via
also reported by Zhang et al. [54] and Delacourt
field-emission scanning electron microscopy
et al. [55]. This significant change in morphology
(FESEM) and the composition of composite
will also make different trend in the corrosion
coatings was evaluated by energy dispersive
behavior of zinc matrix nanocomposite coatings
spectroscopy (EDS) analysis. The weight percent
that will be discussed later. By increasing the
of both elements Zn and Ti in the composite
current density, a rise in applied energy of ions is
coating specimens were analyzed by EDS and
occurred, and accordingly results into the
then volume percentage was calculated using
increased reduction rate of ions. As a result,
densities of zinc (7.13 g/cm3) and nano TiO2
according to Figures 6a to 6c the number of
powder (4.23 g/cm3). It is worth mentioning that
flakes is growth and their size is reduced
the EDS measurements were applied three times
indicating that the area of grain boundaries has
and the average amount was reported for each
been increased.
sample.

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Figure 5. FESEM images of zinc deposited coatings deposited at different current densities: a) 0.08, (b) 0.1, and
(c) 0.12 A/cm2.

Figure 6. FESEM images of Zn-TiO2 composite coating deposited under current densities of: (a) 0.08 A/cm2, (b)
0.1 A/cm2, and (c) 0.12 A/cm2.

Figure 7. (a and b) FESEM images of Zn-TiO2 (10 g/L) nanocomposite coatings electrodeposited under the
current density of 0.12 A/cm2 and (c) EDS measurement.

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Regarding the volume percent of incorporated In Figure 8, it is observed that by rising the
nanoparticles in the composite coating, it should concentration of dispersed nanoparticles in the
be noted that by rising the current density, the electrolyte from 5 to 15 g/L, the content of
alteration in morphology depends on the volume incorporated TiO2 nanoparticles in the coating
percentage of nanoparticles participated in the was steadily decreased. In spite of the decrement
coating. Thus, it can be concluded that the in incorporated particle content in Figure 8 (b
number of participated nanoparticles in the zinc and c), the microstructure of these figures has
matrix coating has two major influences: (i) the same smoothness and uniformity as Figure
reduction in crystallite size and (ii) formation of 8a and also there is a more uniform structure
a more uniform and smoother surface. Figure 6b with smaller crystallites (see Figure 8c) due to
shows more obvious and smaller flakes and, has more uniform distribution of TiO2 nanoparticles
a greater number of flakes and also has a at the concentration of 10 and 15 g/L, so this can
smoother and more uniform surface than Figure form a more uniform and smoother coating in
6a and 6c. This is due to higher content of spite of less incorporated particle content in the
incorporated particles in Figure 6b (current coating. These parameters also affect the
density of 0.1 A/cm2). As mentioned, the highest corrosion behavior which will be discussed later.
amount of incorporated TiO2 in the As mentioned, by increasing the concentration of
nanocomposite coating is related to the sample TiO2 nanoparticles in the electrolyte under a
coated at 0.1 A/cm2 current density. Under the constant current density, the content of
current density of 0.08 A/cm2, Zn 2+ ions have a incorporated nanoparticles in the coating
lower mobility than 0.1 A/cm2 and this results in instantly reduces owing to the lower electrical
the lower incorporation of particles into the charge for each nanoparticle according to the
coating. By enhancing the level of current density constancy of ion concentration in the solution
to 0.1 A/cm2, the mobility of Zn2+ ions increases associated with increasing the particle
and results in more incorporated particles into concentration in the electrolyte. It should also be
the coating. However, by further rising the noted that according to Guglielmi
current density to 0.12 A/cm2, the volume electrodeposition model [57], by increasing the
percentage of incorporated particles decreases particle concentration in the electrolyte, surface
due to the higher mobility of ions than particles. adsorption of particles on cathode, and the
The similar result have been obtained by Stojak volume percent of incorporated particles into the
et al. [56]. EDS measurements were also applied coating initially increases. As a result, it is
to confirm the participation of TiO2 nanoparticles guessed that this rise in volume percent occurs
in the zinc matrix. These measurements also from 0 to 5 g/L concentration of TiO2
determine the composition of composite coatings nanoparticles which has not been studied in this
and the amount of participated TiO2 investigation.
nanoparticles into the zinc matrix. Figure 7
shows the FESEM images and EDS measurement The Analysis of X-ray Diffraction (XRD)
of Zn-TiO2 sample deposited at the concentration
The patterns of XRD analysis of pure zinc and
of 10 g/L TiO2 nanoparticles and
Zn-TiO2 nanocomposite coatings are illustrated
electrodeposited under the current density of
in Figure 9. In the XRD patterns of both coatings,
0.12 A/cm2.Figure 8 shows the FESEM images of
characteristic peaks of Zn such as (002), (100),
Zn-TiO2 nanocomposite coatings deposited at
(101), (102), (103), (004), and (112) planes have
variant concentrations of nanoparticles in the
been recognized. Through adding TiO2
solution.

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nanoparticles into the zinc-based coating, most of addition of H3BO3 and SDS during the
the characteristic peaks experienced a electrodeposition process which is completely
considerably reduced intensity. discussed in other studies [14, 58, 59]. Figure 9
Based on our understanding, this could be describes the XRD patterns of pure Zn and Zn-
originated from the impurity effect due to the TiO2 coatings.

Figure 8. FESEM images of Zn-TiO2 nanocomposite coatings under constant current densities of 0.12 A/cm2 and
particle concentrations in the electrolyte: (a) 5, (b) 10, and (c) 15 g/L.

Figure 9. The XRD patterns of pure zinc and Zn-TiO2 nanocomposite coating electrodeposited at current density
of 0.12 A/cm2, a) pure zinc and b) Zn-TiO2 (5 g/L).

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According to the XRD patterns in Figure 9, the corrosion resistance. Besides, the coating
incorporation of TiO2 nanoparticles has played a stability was intensified in corrosive
significant role on the reduction of relative environment. The addition of TiO2 nanoparticles
intensity of all characteristic peaks justifying that in the electrodeposition process of zinc on the
crystal growth on all crystallographic planes has surface of low carbon steel substrate,
been diminished. The decrease in peaks relative significantly improves the corrosion resistance
intensity and in consequence the crystal growth owing to the TiO2 role and the reinforcement
reduction which is also reported in other studies effect of TiO2 nanoparticles in the nanocomposite
[54,55] is in consistence with our SEM studies in coating.
section 3.1, indicating the grain refinement and
decrement in grain size. Salt Spray Method (Salt Fog Testing)

The Weight Loss Measurements Salt Spray technique is an industrial and also
practical method for estimation of the service life
The profiles of corrosion rate regarding pure of electroplated zinc deposits. In this test, the
zinc and Zn-TiO2 (5 g/L) nanocomposite coated coated specimens were exposed to the vapors or
specimens immersed in 3.5 wt.% NaCl solution fog of 5 wt.% NaCl solution. The fog or drops
for 216 hours were obtained, as depicted in accumulate on the specimens’ surface and
Figure 10. The obtained findings exhibited the accelerates the corrosion. This results into
superior corrosion resistance of Zn-TiO2 appearance of zinc salts called white rust.
nanocomposite coatings in comparison to that of Afterwards, the corrosion resistance of coated
the pure zinc coating. The amount of corrosion specimens was evaluated by the number of hours
rate in Zn and Zn-TiO2 nanocomposite coatings taken for the formation of white rust. The higher
was constant during the entire period of 9 days. corrosion resistance leads to later production of
The results illustrated that the presence of TiO2 white rust and thus the time for formation of
nanoparticles in zinc matrix, varies the corrosion corrosion products is increased. In this research,
behavior of zinc and the nanoparticles the pure zinc exhibited the white rust after 24
embedment leads to improvement of the hours and Zn-TiO2 (5 g/L) nanocomposite after

Figure 10. Variations of corrosion rate with immersion time for pure zinc coating and Zn-TiO2 nanocomposite
coating (5 g/L) samples in 3.5 wt. % NaCl solution (specimens electrodeposited under the current density of 0.12
A/cm2).

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72 hours (both specimens electrodeposited related to the deposition parameters and also
under the current density of 0.12 A/cm2). The shape, size, and characteristics of co-deposited
results of this test prove the superior corrosion particles. Defects, cracks, gaps, crevices, and
resistance of Zn-TiO2 nanocomposite coating micro-holes are non-deniable on the metal
with comparison to pure zinc coating under the surface. Nanoparticles are easily entered into
specified mentioned conditions. these defects leading to change the corrosion
mechanism from localized to more uniform type.
Electrochemical Measurements In the present study, the defects are covered and
filled by TiO2 nanoparticles on the zinc surface.
Anodic Polarization Test
Besides this, these micro-holes act as active sites
for metal dissolution during the corrosion
The anodic polarization measurements of pure
process. As a result, by covering these holes with
zinc coating and Zn-TiO2 (deposited at the 5 g/L
TiO2 nanoparticles in the nanocomposite coating,
concentration of TiO2 nanoparticles)
it will cause a reduction in corrosion and
nanocomposite coating electrodeposited under
dissolution of metal into a corrosive electrolyte.
the current density of 0.12 A/cm2 were measured
in the salt solution with 3.5 wt. % NaCl and
Potentiodynamic Polarization Test
reported in the curve illustrated in Figure 11.
Accordingly, the potential of Zn-TiO2 To have a deeper understanding of corrosion
nanocomposite coating is more positive than that characteristic of pure zinc and Zn-TiO2
of pure Zn coating at all amounts of electric nanocomposite coatings, potentiodynamic
currents. polarization test was applied under the specific
For nanocomposite coating, by increasing the mentioned conditions. The important corrosion
current density, the anodic polarization potential parameters like corrosion potential or Ecorr,
is risen and moves toward the positive direction. corrosion current density or icorr , and anodic and
Electrochemical results show that under cathodic Tafel constants (βa and βc) are extracted
mentioned conditions, Zn-TiO2 nanocomposite from potentiodynamic polarization curves and
coating exhibits lower activity than that of pure summarized in Table 3.
Zn coating. Thus, they show better stability to the
external environment. It should also be stated
that by increasing the potential, the corrosion
current values also increase. Likewise, the
corrosion current value for the Zn-TiO2
nanocomposite coating is lower than that of pure
zinc coating at the same potential.
The effect of nanoparticles participation in the
coating on the corrosion resistance has been
studied by different researchers. For instance,
Shibli et al. [60] studied the high corrosion
resistance of hot dip galvanic zinc reinforced
with TiO2. Lei Shi et al. [61] also reported that the
Figure 11. The anodic polarization curves for pure
corrosion resistance was increased by the
zinc coating and Zn-TiO2 (5 g/L) nanocomposite
addition of SiC nanoparticles into the Ni-Co coating electrodeposited under the current density of
alloys. These results indicate that the corrosion 0.12 A/cm2 in NaCl solution (3.5 wt.%).
resistance of nanocomposite coatings is highly

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Table 3. Corrosion characteristics and TiO2 content of the coatings

βa
TiO2 i Ecorr icorr βc TiO2 (Vol.
Coating (mV. rcorr (mpy)
(g/L) (A/cm2) (mV) (µA/cm2) (mV. decade-1) %)
decade-1)

Zn 0 0.08 -1.11 9.57 0.005 0.008 0 5.7

Zn 0 0.10 -1.12 51.7 0.005 0.006 0 30.8
Zn 0 0.12 -1.06 9.65 0.004 0.004 0 5.8
Zn-TiO2 5 0.08 -1.09 265 0.005 0.008 2.22 159.4
Zn-TiO2 5 0.1 -1.08 93.3 0.005 0.0059 2.93 56.3
Zn-TiO2 5 0.12 -1.05 2.7 0.004 0.004 2.48 1.6
Zn-TiO2 10 0.12 -1.04 11.9 0.006 0.005 1.14 7.1
Zn-TiO2 15 0.12 -1.02 40.5 0.004 0.005 0.43 24.3

For pure zinc coatings, as shown in Table 3, by from 0.08 to 0.1 A/cm2, the incorporation rate of
increasing the current density from 0.08 to 0.1 TiO2 nanoparticles in the coating was enhanced
A/cm2, Ecorr (corrosion potential) is and leads to improvement of corrosion
approximately constant and icorr (corrosion resistance of composite coating. This behavior is
current density) is also increased. The rise in icorr the result of mechanism regarding corrosion
is due to reduction in zinc crystallite size and also improvement in composite coatings that occurs
enhancement of the grain boundaries between for two essential reasons:
these crystallites resulting in more exposed 1. Participation of TiO2 nanoparticles into the
corrosion sites in the microstructure [53]. By zinc matrix results in the formation of several
increasing the current density from 0.1 to 0.12 corrosion micro cells in which, inert TiO2
A/cm2, icorr decreases which is in agreement with nanoparticles act as cathode and zinc matrix also
increase in Ecorr. The decrease in icorr or higher acts as anode due to the higher electrochemical
corrosion resistance in this range is mainly potential of TiO2 than zinc metal matrix. Thus,
ascribed to the formation of a more uniform and such corrosion micro cells accelerate the anode
compact microstructure (Figure 5) while the matrix polarization and result in the formation of
amount of grain boundaries between hexagonal passive sites.
zinc crystals is risen. As a result, it can be 2. Inert TiO2 nanoparticles act as physical
concluded that for analysis of icorr obtained for barriers to corrosion environment through
zinc deposited coatings, two main factors are of microstructure modification. This occurs by
importance: (i) the amount of grain boundaries filling the gaps and defects at the surface by TiO2
between hexagonal zinc crystals (if this nanoparticles. As a matter of fact, in the presence
overcomes, icorr is increased) and (ii) the amount of TiO2 nanoparticles, localized corrosion
of uniformity and compactness of surface converts to uniform corrosion that is more
morphology (if this overcomes, icorr is decreased). predictable and possible to control [61,62].
For Zn-TiO2 nanocomposite coatings, as shown For Zn-TiO2 nanocomposite coatings, by rising
in Table 3, by rising the current density, icorr is the current density from 0.1 A/cm2 to 0.12
steadily lowered indicating the improvement of A/cm2, although the amount of the TiO2
corrosion resistance. The main point here is that nanoparticles incorporated in the coating is
by rising the electrodeposition current density lowered and as a result the corrosion resistance

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is improved. In other words, despite the decrease with reinforced particles, in this case for TiO2
in the incorporated nanoparticles, rising the nanoparticles, will not necessarily increase the
current density as a proportional factor with ions corrosion resistance. The rise or fall of corrosion
reduction rate or the driving force for movement resistance is highly relied on the influence (e.g.,
of ions toward cathode, the corrosion resistance amount and distribution) of incorporated
is risen owing to the formation of more uniform particle into the matrix. In case of zinc metal
and compact microstructure. Therefore, two matrix coatings, as mentioned previously, the
important factors have great influence on the zinc morphology can alter drastically from
corrosion characteristics of the nanocomposite hexagonal platelet to flake type grain
coatings: (i) the incorporated rate of microstructure after incorporation of TiO2
nanoparticles making the composite surface nanoparticles.
smoother and (ii) the level of electrodeposition As demonstrated in Figures 6 to 8, the
current density affecting the uniformity and morphology of electrodeposited Zn-TiO2
compactness of composite coatings. nanocomposite coatings are almost flake type
For Zn-TiO2 nanocomposite coatings, according grains. This type of morphology is the result of
to Table 3, the corrosion current density (icorr) significant grain refinement and possess much
was recorded to be lower than the pure Zn higher grain boundaries than hexagonal platelet
coating deposited under the 5 g/L concentration microstructure which is more observed in pure
of TiO2 nanoparticles. By increasing the zinc coatings. This presence of higher amount of
concentration of TiO2 nanoparticles in the grain boundaries makes the coating more
electrolyte from 5 to 15 g/L, icorr was significantly susceptible to corrosion.
increased. In fact, at constant current density, icorr It is eventually observed that between all pure
was highly relied on the function of incorporated and composite deposited coatings (see Table. 3),
particle content in the coating. Thus, according to the electrodeposited Zn-TiO2 (5 g/L) coating at
the further reduction in participation rate of TiO2 the current density 0.12 A/cm2 exhibited the
nanoparticles under the 10 and 15 g/L lowest amount of icorr (equals to highest
concentration of TiO2 nanoparticles, the corrosion resistance) of 2.7 µA/cm2 equals to 1.6
corrosion resistance was steadily lowered than mpy. It is noteworthy that in this study, the
that of the sample deposited at concentration of electrodeposited Zn-TiO2 (5 g/L) coating at the
5 g/L in the same condition of deposition. current density 0.12 A/cm2 has the highest
This increased distribution of nanoparticles and corrosion resistance between all pure and
coating uniformity is also observed in FESEM composite deposited coatings. In case of
images illustrated in Figure 8. Accordingly, by industrial applications of zinc-based coatings, the
increasing the particle concentration in the lowest icorr is not always the best choice for
electrolyte, the distribution of nanoparticles and application of a specific coating, since the
uniformity of the coating has risen, and also protection mechanism of zinc is acting as a
resulted in formation of a more uniform sacrificial coating and should be corroded in
microstructure and a greater number of flakes of order to protect its substrate from corrosive
smaller size. environment. Thus, in case of industrial
By assessing the data reported in Table 3, for applications of zinc-based coatings, the choice of
several conditions, icorr is higher for Zn-TiO2 coating between various deposition parameters
nanocomposite coating with respect to that of the depends on the different parameters like desired
pure Zn coating. This clearly indicates the lifetime and the constituents of corrosive media.
electrodeposition of nanocomposite coatings

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Figure 12. Corrosion rates (mpy) of the pure zinc and Zn-TiO2 nanocomposite coatings under variant
electrodeposition current density and TiO2 nanoparticle concentration.

The corrosion rates (C.R) versus mpy for pure Zn nanocomposite coating, the corrosion product
and Zn-TiO2 nanocomposite coatings were sites have a smaller size than that of pure zinc
calculated by following equation: coating.

Corrosion Rate (mpy) = 0.13 (1)

Where, M (g) describes molar mass, n denotes

the charge number, and d (g/cm3) indicates the
density of zinc. The values of the corrosion rates
of the pure Zn and Zn-TiO2 nanocomposite
coating specimens are calculated and illustrated
in Figure 12.

Morphology after Corrosion

To have a full assessment of coatings

morphology, the pure zinc and Zn-TiO2 (5 g/L)
coated specimens electrodeposited under the
current density of 0.12 A/cm2 were subjected
into the chemical corrosion process in 3.5 wt.%
NaCl solution for 9 days. The corroded samples
were used to take FESEM images as indicated in
Figures 13 and 14. The FESEM images of the
corroded specimens demonstrates the less
corrosion resistance of pure zinc coating than Figure 13. FESEM images for pure zinc coating
that of the corroded Zn-TiO2 nanocomposite specimens (electrodeposited under the current
coating. density of 0.12 A/cm2) after 9 days weight loss
It is also obvious that in the mentioned measurements at two different magnifications.
conditions, nanocomposite coating exhibits more
uniform corrosion whereas pure zinc coating
exhibits more localized corrosion. In case of

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to that of the pure zinc coating. The rise of

corrosion resistance is originated from the
physical barrier produced by TiO2 against the
corrosion process through filling crevices, gaps
and micro holes on the surface of zinc coating.
The uniformly distributed TiO2 nanoparticles,
until the critical concentration, resulted into the
increment of the corrosion potential value
toward the more positive values for Zn-TiO2
nanocomposite coating and in consequence
higher corrosion resistance. The nanocomposite
coatings depicted more uniform corrosion.
In this study, the use of TiO2 nanoparticles has
been investigated to control of zinc coating
corrosion, and also the electrolyte could generate
Zn-TiO2 nano composite coatings at larger scales.
Increase in the electrodeposition current density
from 0.08 to 0.12 A/cm2 for both pure Zn and Zn-
TiO2 nanocomposite coatings, led to higher
Figure 14. FESEM images for Zn-TiO2 (5 g/L)
nucleation rate, reduction rate of ions, and also
nanocomposite coating specimens (electrodeposited
under the current density of 0.12 A/cm2) after 9 days
reduction in crystal growth was occurred which
weight loss measurements at two different subsequently led to deposit more and smaller
magnifications. crystals. By participation of TiO2 nanoparticles in
the coating, the morphology was changed
This shows the higher rate of corrosion in the drastically from hexagonal platelet crystals to
pure zinc coating than Zn-TiO2 nanocomposite flake type grains causing remarkable grain
coating, and also validates the former corrosion refinement and reduction in crystal growth
resistance measurements. The FESEM studies observed by FESEM and confirmed by XRD.
further confirms the obtained results of the Due to the further rising of TiO2 nanoparticles
weight loss and polarization tests. concentration from 5 to 15 g/L, the
incorporation rate of TiO2 nanoparticles had
Conclusion gradually decreased, and grain refinement
associated with more uniform surface was
In this research, Zn and Zn-TiO2 nanocomposite
observed at 15 g/L TiO2 concentration. Weight
coatings were successfully prepared by electro-
loss measurements, salt spray tests, and anodic
codeposition method. The TiO2 nanoparticles
polarization test indicated the higher corrosion
were dispersed uniformly in the solution and
resistance of Zn-TiO2 (5 g/L) than that of the
included in the zinc coating during
pure Zn coating electrodeposited under the
electrodeposition. The incorporation of TiO2
current density of 0.12 A/cm2. Potentiodynamic
nanoparticles in the coating resulted into
polarization results showed that rising the
reduction of the crystal size and also until a
current density from 0.08 to 0.1 A/cm2, icorr was
critical concentration, led to remarkable
increased for pure zinc coating, then a decrease
improvement of the corrosion resistance
from 0.1 to 0.12 A/cm2 occurred. However, for
regarding the nanocomposite coatings compared
Zn-TiO2 coating by increase in current density

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HOW TO CITE THIS ARTICLE

Mohammad Sajjadnejad*, Sara Karkon, Seyed Mohammad Saleh Haghshenas. Corrosion Characteristics of Zn-TiO2
Nanocomposite Coatings Fabricated by Electro-Codeposition Process. Adv. J. Chem. A, 2024, 7(2), 209-226.
DOI: 10.48309/ajca.2024.418391.1425
URL: https://www.ajchem-a.com/article_184854.html

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