{Anticorrosive polystyrene coatings modified with tannic acid on zinc and steel substrates:}
http://dx.doi.org/10.5599/jese.1293 721
J. Electrochem. Sci. Eng. 12(4) (2022) 721-730 http://dx.doi.org/10.5599/jese.1293
Open Access : : ISSN 1847-9286
www.jESE-online.org
Original scientific paper
Anticorrosive polystyrene coatings modified with tannic acid on
zinc and steel substrates
Julia Both1, Gabriella Stefánia Szabó2,, Gabriel Katona2 and Liana-Maria Mureșan1
1Babeş-Bolyai University, Faculty of Chemistry and Chemical Engineering, Department of Chemical
Engineering, RO-400028, Cluj-Napoca, Romania
2Babeş-Bolyai University, Faculty of Chemistry and Chemical Engineering, Department of Chemistry
and Chemical Engineering, Hungarian line of study, RO-400028, Cluj-Napoca, Romania
Corresponding author: gabriella.szabo@ubbcluj.ro
Received: February 26, 2022; Accepted: May 20, 2022; Published: June 7, 2022
Abstract
Polystyrene (PS) polymer layers were prepared by the sol-gel method and studied as anticorrosive
barrier layers on carbon steel and zinc substrates. To increase the corrosion resistance of the
coatings, two different approaches were considered: (i) the use of mesoporous silica-nano-
containers impregnated with a corrosion inhibitor (tannic acid) introduced into the polystyrene
matrix and (ii) direct impregnation of polystyrene coatings with the same corrosion inhibitor. The
impregnated nanocontainers were characterized by transmission electron microscopy. The
thickness and the adhesion of the coatings were measured, and their corrosion behavior was
investigated by electrochemical impedance spectroscopy. Results showed that the used inhibitor
slightly decreased adhesion, but significantly increased the corrosion resistance of the coatings.
The direct introduction of tannic acid into the polymer matrix offers higher corrosion resistance
than in the case of polystyrene coatings doped with impregnated silica nanocontainers.
Keywords
Polystyrene coatings; corrosion protection; tannic acid; mesoporous silica nanocontainers
Introduction
Corrosion is an inevitable phenomenon in the gradual deterioration of metals because of
aggressive environments and researchers are constantly preoccupied with preventing or minimizing
it [1]. Methods of anticorrosion protection include the production of metal alloys (active protection)
and the application of corrosion barrier layers on metals surface (passive protection). Aiming to avoid
health issues and environmental problems, the production of chromate-free coatings [2] and
harmless, effective organic and inorganic barrier coatings [3,4] on metals have taken the place of
previously performant technologies having carcinogen nature and general toxicity [5].
Styrene, alongside a plethora of polymerizing agents forms polystyrene (PS), a vinyl polymer
composed of a long hydrocarbon chain with phenyl groups attached to every other carbon atom.
The most common use of polystyrene is in the production of plastics [6], and since it exhibits
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interesting thermic characteristics, it is the precursor of Styrofoam, a material widely used in various
industries. In the corrosion protection domain, PS has mainly been used in the form of copolymers
with different acids [7] or the form of a copolymer with cornstarch [8] for the corrosion protection
of steel substrates. PS microcapsules containing silanol and Ce (III) inhibitors in epoxy coatings have
also been reported as corrosion barrier systems [9]. PS, as any other coating matrix offers, the
possibility of improvement by the addition of corrosion inhibitors.
Reported examples of corrosion inhibitors for steel and zinc are rare earth salts (such as CeCl3 or
LaCl3) [10], organic compounds, such as benzotriazole [11], and gallotannins [12] such as gallic acid
and tannic acid, with rust converter characteristics. Tannic acid, a safe, non-toxic and
environmentally friendly polyphenolic compound, forms complexes with the surfaces of the metal
substrates generating an additional corrosion preventive thin film on the metallic structures [13].
These complex-forming characteristics of gallotannins, especially of tannic acid, make them eligible
as inhibitors for the preparation of corrosion-resistant coatings.
Nanocontainers are widely used as corrosion inhibitor carriers in various systems. These nano-
particles offer ingenious solutions for the preparation of self-healing coatings by their versatility and
the capability of controlled release of incorporated inhibitors. Previous studies discuss the appli-
cation of urea-formaldehyde microcapsules filled with epoxy resin for self-healing coatings on steel
substrates [14]. Mesoporous silica nanoparticles loaded with molybdate [15] or 2-mercaptoben-
zothiazole [16] were also reported for the corrosion protection of aluminum and steel alloys. The
silica nanocontainers have also been reported in combination with tannic acid, used as a sealing
agent, for benzotriazole impregnated mesoporous particles [17].
As mentioned above, applications of silica nanoparticles are widely discussed as inhibitor carriers
in various coating systems. Following that thought pattern, we aimed to study whether the
introduction of tannic acid in the nanocontainers versus the direct introduction into the coating
would have a more beneficial effect on the PS coating, which by itself had a measly protective effect.
Consequently, the aim of this study was the preparation of protective PS polymer coatings on zinc
and steel substrates in the absence and in the presence of tannic acid as a corrosion inhibitor. The
novelty of the research consists in the comparison between the characteristics of PS coatings
prepared on zinc and mild steel by dip-coating, using two different approaches: (i) direct addition of
tannic acid into the sol before polymerization of styrene and (ii) addition of tannic acid impregnated
silica nanocontainers into the sol. The coatings were characterized by electrochemical impedance
spectroscopy (EIS), the synthesized mesoporous nanocontainers were analyzed by transmission
electron microscopy (TEM), and the prepared coatings were also subjected to adhesion and coating
thickness measurements.
Experimental
Materials and methods
Zinc and mild steel substrates were used as metal substrates for the produced coatings. The used
metal wafers were pre-treated: firstly, both metal substrates were abraded with rougher emery
papers in the range of 800-1500, then polished with fine emery papers (grain size in the range of
2000-5000) followed by a degreasing step, prior to the application of the coatings.
Polystyrene sol was prepared from the 1:2 ratio of Syntevene-404 (GALLSTAFF MULTIRESINE) and
Dibenzoyl peroxide 97 % (ALFA-AESAR). Mesoporous silica nanocontainers were synthesized from
the mixture of tetraethyl orthosilicate (SIGMA-ALDRICH), absolute ethanol 99.9 % (SIGMA-ALD-
RICH), cetyltrimethylammonium bromide 98 % (SIGMA-ALDRICH), and sodium hydroxide 97 %
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(ACS REAGENT). Tannic acid (SIGMA-ALDRICH), as a corrosion inhibitor, was introduced in 1 wt.%,
separately into the coating matrix, respectively into the synthesized silica nanocontainers.
Protective coatings were prepared using a homemade dip-coater. Electrochemical measure-
ments were effectuated on a AUTOLAB 302, with the use of a three-electrode cell in 0.2 g/L Na2SO4
(SIGMA-ALDRICH) electrolyte solution. The three-electrode cell consisted of a working electrode
(zinc and mild steel substrates), a counter electrode (platinum wire) and a reference electrode
(Ag/AgCl/KClsat).
TEM measurements were performed on a H-9500,100-300 kV HITACHI HIGH-TECH GLOBAL
machine. Adhesion was measured with a TQC ADHESION TEST KIT while coating thickness measure-
ments were effectuated with the use of an ELMATRONIC F / NF -1250 μm measuring instrument.
Synthesis of silica nanocontainers
0.5 ml of 2 M NaOH was added to a mixture of 0.5 g of CATB and 70 ml of water. The mixture was
then heated to 80 °C and 4 mL of TEOS was added with continuous stirring. After stirring at 80 °C for
two hours, an opaque, milky solution was obtained. The precipitated solution was filtered, following
which the filtrate was rinsed with distilled water (2×5 mL) and ethanol (2×5 mL). After drying in an
oven for approx. 24 hours, the filtration was sintered at 600 °C for 5 hours. The process leads to
obtaining mesoporous silica nanocontainers.
Parts of the nanocontainers were added to an aqueous tannic acid solution, for impregnation.
The nanocontainers were kept for 1 hour in the 1 wt.% tannic acid solution before being filtered and
washed with both water and ethanol to remove the tannic acid from the exterior of the mesoporous
silica particles.
Transmission electron microscopy measurements
Transmission electron microscopy (TEM) measurements were performed on the mesoporous
silica nanocontainers with a H-9500,100-300 kV HITACHI HIGH-TECH GLOBAL measuring instrument.
TEM analysis served to determine the diameter of the silica nanocontainers in order to establish
whether the tannic acid molecule fits on the inside of the mesoporous silica particles.
Preparation of polystyrene precursor
Four different styrene precursor solutions were prepared. The four different solutions were
based on a 1:2 mixture of styrene and its polymerizing agent, dibenzoyl peroxide. One solution was
left for a polystyrene layer reference (PS); in the second, nanocontainers were added in a concen-
tration of 1 % (PS+NC); tannic acid was added in a concentration of 1 % to the third (PS+TA), and
nanocontainers impregnated with 1 % tannic acid (PS+TA+NC) were added to the last solution. In
every case, following the addition of filler substances, the PS sol was placed in an ultrasonic bath for
approximately 15 minutes to ensure desolvation and avoid agglomeration of the aforementioned
substances. All four precursor solutions, based on preliminary studies, were allowed to polymerize
for 10 days until they reached the optimum viscosity for layer drawing.
Preparation of coatings on zinc and mild steel substrates
For both metal substrates, the same pretreatment steps were followed: the first step of the
pretreatment was the sanding, followed by the degreasing of the metal wafers. The zinc plates were
polished using a polishing machine and an organic-based polishing paste, then degreased in
hydrochloric acid, rinsed with distilled water, sonicated in alcohol, and finally dried. In the case of
mild steel sheets, as they proved to be more delicate to treatment with hydrochloric acid, the
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surfaces were first sanded with coarser sandpaper, then thoroughly washed with a detergent
containing caustic soda, in order to get the pre-existing paraffin coating, of the mild steel, off. Mild
steel sheets were then rinsed in alcohol and dried in a manner similar to the zinc substrates.
The layers were applied to the metal surfaces by the dip-coating method. Two samples were
prepared from each of the four sols to monitor reproducibility. The layers were drawn at a rate of
12 cm min-1. After layer drawing, thermal treatment at 80 °C for one hour was applied until the
polymerization process was complete. The end of the polymerization was indicated by the
hardening of the layer.
Adhesion and layer thickness measurements
The adhesion measurements were performed with a robust grating cutter with an aluminum
head, with replaceable blades called a TQC ADHESION TEST KIT. The cutter had self-aligning blades
that followed the line of the surface. A symmetrical square mesh was scratched into the metal
substrate. Subsequently, a special adhesive tape meeting international standards was placed on the
scratched surface of the plate. The number of incised squares remaining intact on the surface versus
the number of squares that ripped off with the tape came up with the tape, the percentage of
adhesion was calculated using the Lattice-Notch formula according to certain standard tables.
The layer thickness was determined using an instrument that is able to read coating thicknesses
on both metallic and non-metallic surfaces by magnetic induction or eddy current method for layers
of any origin, namely an ELMATRONIC F / NF -1250 μm measuring instrument. Placing the apparatus
perpendicular to the layered metal surface, layer thickness values for each of our different types of
layers were determined.
Wettability measurements
Wettability measurements were carried out by the sessile-drop method on all substrates and
coatings mentioned. The measurements were made by adding a 20 µl electrolyte droplet of 0.2 g/L
Na2SO4 electrolyte solution of pH 5, in a saturated Na2SO4 vapor atmosphere. The resulting images
were processed, and contact angle determination was made in ImageJ software (developed by
Wayne Rasband).
Electrochemical characterization of the coatings
Electrochemical measurements were performed on a PARSTAT 227 potentiostat, using a three-
electrode cell consisting of a working electrode (zinc and mild steel wafer), counter electrode (Pt
wire) and a reference electrode (Ag/AgCl/KClsat) immersed in 0.2 g/L sodium sulphate (SIGMA-
ALDRICH) (pH 5) electrolyte solution. The layers were firstly characterized by open-circuit potential
measurements (OCP) in order to determine the resting potential values of both the coated zinc and
mild steel samples. OCP measurements were left to stabilize for 60 minutes each and offered a
benchmark for all further electrochemical characterization.
In a further study, electrochemical impedance spectroscopy (EIS) measurements were performed
in the 10 mHz to 100 kHz frequency range with the use of a sinusoidal current (10 mV).
Results and discussion
Transmission electron microscopy analysis
Previously prepared silica nanocontainers were subjected to TEM analysis and the obtained
images are shown in Figure 1. The purpose was to get information about the shape and diameter of
the particles and to determine if they belonged to the nano range at all. Furthermore, we also
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wanted to know whether the inhibitor molecule, more specifically the tannic acid molecule fits in,
given that it is a molecule of 1.85×1.65×1.01 nm [18]. Based on the TEM images, we can state
without any doubt that the diameter of the nanocontainers is in size range of 20 to 50 nm. This
would theoretically allow the tannic acid molecule to be hosted by the nanoparticles.
Figure 1. Transmission electron microscopy images reflecting a cluster of synthesised mesoporous silica
nanocontainers at scales of (A) 200 nm respectively (B) 50 nm
Adhesion and coating thickness evaluation
Prior to the application of the PS-based layers and the measurement of their adhesion to the
substrate, the surface of the plates was subjected to thorough cleaning and polishing operations.
All these procedures were required in order to presumably promote a high level of adhesion of the
protective coating. The purpose of measuring the adhesion was to obtain information about the
quality of a protective coating, more precisely, how and to what extent it has established a high-
quality, long-lasting adhesion to the sheet to be protected. If adhesion proves inadequate, electro-
lyte infiltrations may occur beneath the layer, which can cause local corrosion, which is worse than
corrosion that occurs in the complete absence of a protective coating.
Adhesion was quantified by coating type since there were no observed significant differences
between the adhesion of the coatings on the two different metals. To calculate the adherence of
the prepared coating types, the Lattice-Notch equation (1) was applied. In Equation 1, the
parameter a stand for the total of squares meshed into the coating, while b, for the total number of
squares ripped off by the special tape. Adhesion can parallelly be assessed with the help of so-called
ASTM standards [19], which also take into consideration the measure by which the coating gets
damaged following the tearing of the square mesh. These standards come as follows: 5B (no
detachment), 4B (detachment of flakes, a maximum of 5 % damage), 3B (coating flaking around the
edges, less than 15 % damage), 2B (detachment of ribbons with the cuts and squares, damage less
than 35 %), 1B (greater detachment of the coating along the cuts, part of the squares gone, damage
lesser than 65 %) and 0B (flaking that cannot be classified).
Adhesion 100
a b
a
−
= (1)
It can be observed from Table 1 and Figure 2 that the presence of tannic acid, although slightly
reduces adhesion for both substrate types.
The obtained adhesion results can be explained by the fact that the formation of metal tannates
on the metal surface by a reaction between TA and the metal is a faster process than the
polymerization of polystyrene. If so, the polystyrene adheres to an intermediate porous layer
formed by a complex of iron or zinc oxides and tannic acid [13], which leads to poorer adhesion.
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A
B
C
D
E
F
G
H
Figure 2. Adhesion tests performed on both mild steel and zinc substrates coated with the following layers:
(A) Zn PS, (B) Zn PS+NC, (C) Zn PS+TA, (D). Zn PS+TA+NC, (E) mild steel PS, (F) mild steel PS+NC,
(G) mild steel PS+TA, (H) mild stel PS+TA+NC
The layers thicknesses were determined for all the investigated coatings using an instrument that
is able to read layer thicknesses on surfaces by magnetic induction or the eddy current method. The
results are presented in Table 1 and show that the addition of NC or TA in the PS layer leads to an
increase of the coating thickness, which is approximately the same in all cases, around 20 µm.
Table 1. Results of adhesion and layer thickness evaluation for the PS, PS+NC, PS+TA and PS+TA+NC coatings
on zinc and mild steel substrates
Sample Layer thickness, µm Adhesion, % Adhesion class (ASTM)
Zn/PS 8.0 95 4B
Zn/PS+NC 20.0 95 4B
Zn/PS+TA 21.8 91 3B
Zn/PS+TA+NC 21.8 87 3B
Mild steel/PS 8.0 ∼85 2B
Mild steel/PS+NC 20.0 ∼ 65 1B
Mild steel/PS+TA 21.8 ∼85 2B
Mild steel/PS+TA+NC 21.8 ∼85 2B
In the case of the mild steel wafers, the coatings tore to a much greater extent, which led to the
conclusion of a poorer adhesion than in the case of the zinc substrates. An explanation of this phe-
nomenon can be that the mild steel has proven over the course of the experiment to be much more
reactive to any corrosive factor than zinc, which possibly includes the additives of the PS.
Wettability measurements
Wettability measurements were performed on all types of coatings on both zinc and mild steel
substrates. Figure 2 contains the results of wettability measurements and the initial contact angle
values of each coating on both zinc and mild steel substrates. Tannin acid is a plant-derived
polyphenolic substance that is hydrophilic, which explains the lower contact angle noticed in its
presence in the coatings.
Same observation for the silica NC, which also increase hydrophilicity of the coating and thus,
wettability. Nevertheless, the decrease is not a significant one.
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Figure 3. Wettability measurements (at 0 min) effectuated with 20 µl droplet of 0.2 g/L Na2SO4 electrolyte
solution on the following coatings: A. Zn PS, B. Zn PS+NC, C. Zn PS+TA, D. Zn PS+TA+NC, E. Fe PS,
F. Fe PS+NC, G. Fe PS+TA, H. Fe PS+TA+NC
Electrochemical characterization
Figure 4 shows the complex plane representation of the EIS spectra of the various layers
deposited on zinc plates. As expected, the impedance value of the undoped polystyrene layer (PS)
on zinc is higher than the impedance of the bare zinc plate. The presence of the empty silica
nanocontainers in the polymeric coating (PS + NC) ruins the impedance of the PS by lowering its
impedance values beneath those of the bare zinc plate. The nanoparticles seem to act as defects of
the coating, favoring corrosion. Low compatibility between PS and silica can also explain the poor
corrosion resistance of (PS+NC) coatings.
Figure 4. EIS plots of the Zn ref, PS, PS+NC, PS+TA, PS+TA+NC coatings on Zn substrates in
0.2 g/l Na2SO4 solution (pH 5)
In the next step, silica nanocontainers impregnated with tannic acid were introduced into the
polystyrene layer resulting (PS + NC + TA) coatings, and on the other hand, PS coatings were directly
impregnated with tannic acid (PS+TA).
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The EIS plots corresponding to the different coatings put in evidence the beneficial effect of
tannic acid. Tannic acid is known as an effective anticorrosive agent [20] that reacts with corrosion
products formed on the metal surface and stabilizes them. This characteristic can be observed in
this case as well.
A comparison between the impedance spectra of Zn/(PS + NC +TA) and Zn/(PS+TA) coatings leads
to the conclusion that TA is more effective when it is directly incorporated in PS (a larger capacitive
loop is observed in the latter case). This is probably due to the fact that tannic acid is likely to remain
adsorbed in a higher concentration in PS than in the presence of nanocontainers, which were
washed with water after impregnation and some tannic acid may have been removed during the
process. A second possibility is the better compatibility between PS and TA than between PS and
silica. Compared to the PS and (PS + NC) layers, tannic acid strongly exerted an inhibiting effect both
in the (PS + TA + NC) and the (PS + TA) coatings. It can also be observed that in the presence of TA
in the coatings, the shape of the spectra changes (a second capacitive loop is outlined), suggesting
the change in the mechanism of the corrosion process. Further research and modelling of the
spectra will elucidate this aspect.
Figure 5 presents the impedance spectra of coatings deposited on mild steel substrates coated
with the same aforementioned sols.
Figure 5. EIS plots of the Fe ref, PS, PS+NC, PS+TA, PS+TA+NC coatings on mild steel substrates in
0.2 g/l Na2SO4 solution (pH 5)
The same resistance-improving effect of tannic acid, either embedded in silica nanocontainers or
directly in the polymeric matrix, was observed compared to the undoped PS coating. At the same
time, it should be mentioned that compared to the modified PS layers on zinc, the (PS+TA) and
(PS+NC+TA) layers drawn on mild steel show lower impedance values.
This observation was corroborated with literature data mentioning that tannic acid is a more
efficient inhibitor on zinc than on mild steel [20]. A possible explanation in our case could be the
fact that zinc substrates were much easier to polish in the pretreatment step, resulting in a smoother
surface for the polymeric coating to adhere to. In many cases, zinc has better compatibility with
materials, while mild steel oxidizes extremely quickly and often forms complexes not compatible
with passive corrosion protective methods.
On the mild steel substrates, the end result is the same as in the case of zinc: TA improves the
corrosion resistance of the coatings, and the polystyrene layer impregnated directly with tannic acid
has a higher anticorrosion resistance than that containing the TA modified silica nanocontainers.
0 10000 20000 30000 40000 50000
0
10000
20000
30000
40000
50000
Fe ref
PS
PS+TA+NC
PS+TA
PS+NC
-Z
"
/
Ω
c
m
2
Z' / Ω cm2
0 1000 2000 3000
0
1000
2000
3000
Z' / Ω cm2
-Z
"
/
Ω
c
m
2
Fe ref
PS
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Conclusions
The effect of tannic acid embedded in polystyrene coatings by two different ways on the
anticorrosion protection of zinc and steel was investigated by electrochemical, layer thickness and
adhesion measurements. On the one hand, silica nanocontainers of 20-50 µm diameter were
impregnated with an aqueous solution of tannic acid, then introduced into a polystyrene coating
matrix, and on the other hand, tannic acid was directly introduced into the polystyrene coating in
the sol-preparation step. The results corresponding to doped polystyrene were compared with
those for simple polystyrene coating and polystyrene containing empty silica nanocontainers.
Tannic acid showed an inhibitory effect in both systems compared to polystyrene layers with
empty nanocontainers for zinc and steel. Unfortunately, adhesion is reduced by the presence of
tannic acid. This may be due to the fact that the formation of the tannate complex on the surface
determines polystyrene to bind to an intermediate, porous layer, resulting in poor adhesion of PS
coatings. However, the increased corrosion resistance makes doped PS layers promising candidates
for low-cost, corrosion-resistant protective coatings.
Best corrosion-resistant properties were evident when tannic acid was directly introduced into
the polystyrene coating in the sol-preparation step.
Acknowledgements: Financial support from the program Entrepreneurship for innovation through
doctoral and postdoctoral research POCU/380/6/13/123886 is appreciated. Julia Both thanks for the
financial support from the Romanian Ministry of National Education within her PhD stage.
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@Article{Both2022,
author = {Both, Julia and Szabo, Gabriella Stefania and Katona, Gabriel and Mureșan, Liana Maria},
journal = {Journal of Electrochemical Science and Engineering},
title = {{Anticorrosive polystyrene coatings modified with tannic acid on zinc and steel substrates:}},
year = {2022},
issn = {1847-9286},
month = {jun},
number = {4},
pages = {721--730},
volume = {12},
abstract = {Polystyrene (PS) polymer layers were prepared by the sol-gel method and studied as anticorrosive barrier layers on carbon steel and zinc substrates. To increase the corrosion resistance of the coatings, two different approaches were considered: (i) the use of mesoporous silica-nanocontainers impregnated with a corrosion inhibitor (tannic acid) introduced into the polystyrene matrix and (ii) direct impregnation of polystyrene coatings with the same corrosion inhibitor. The impregnated nanocontainers were characterized by transmission electron microscopy. The thickness and the adhesion of the coatings were measured, and their corrosion behavior was investigated by electrochemical impedance spectroscopy. Results showed that the used inhibitor slightly decreased adhesion, but significantly increased the corrosion resistance of the coatings. The direct introduction of tannic acid into the polymer matrix offers higher corrosion resistance than in the case of polystyrene coatings doped with impregnated silica nanocontainers.},
doi = {10.5599/JESE.1293},
file = {:D\:/OneDrive/Mendeley Desktop/Both et al. - 2022 - Anticorrosive polystyrene coatings modified with tannic acid on zinc and steel substrates.pdf:pdf;:10_jESE_1293.pdf:PDF},
keywords = {Polystyrene coatings, corrosion protection, mesoporous silica nanocontainers, tannic acid},
publisher = {International Association of Physical Chemists (IAPC)},
url = {https://pub.iapchem.org/ojs/index.php/JESE/article/view/1293},
}