Alexandria Engineering Journal (2022) xxx, xxx–xxx

H O S T E D BY
Alexandria University

Alexandria Engineering Journal

www.elsevier.com/locate/aej
www.sciencedirect.com

Preparation of inorganic-polymer nano-emulsion

inhibitor for corrosion resistance of steel
reinforcement for concrete
Ang Zhang, Yixiao Wang *, Huijuan Wang

School of Civil Engineering, Zhongyuan Institute of Science and Technology, Zhengzhou, Henan 451400, China

Received 19 September 2022; revised 4 November 2022; accepted 14 November 2022

KEYWORDS Abstract In this work, the effect of inorganic–organic corrosion inhibitor composition on corro-
Corrosion inhibitor; sion inhibition rate was studied through electrochemical accelerated corrosion experiments and
Steel; ambient atmosphere corrosion experiments. The corrosion inhibitor performance was analyzed
Corrosion inhibition; to establish the relationship between inhibitor composition, steel temperature, inhibitor tempera-
Sodium carbonate; ture, treatment time and corrosion inhibition rate. The effect of nano-emulsion type on the corro-
Fluorocarbon nano- sion inhibition rate of reinforcing steel shows that different types of nano-emulsions can increase the
emulsion self-corrosion potential and reduce the corrosion current of reinforcing steel, improving the corro-
sion resistance of reinforcing steel. The highest corrosion inhibition rate of 72.1% could be achieved
with the addition of fluorocarbon nano-emulsion DF-1 to the corrosion inhibitor. This indicates
that among the studied polymer nano-emulsions, fluorocarbon nano-emulsion DF-1 is the best
polymer nano-emulsion corrosion inhibitor with a better content of 5%.
Ó 2022 THE AUTHORS. Published by Elsevier BV on behalf of Faculty of Engineering, Alexandria
University. This is an open access article under the CC BY-NC-ND license (http://creativecommons.org/
licenses/by-nc-nd/4.0/).

1. Introduction [1–4]. The surface of the steel bar has uneven electrochemical
properties. There are not only anode area with relatively pos-
Corrosion inhibitor is a substance present in the medium in a itive potential, but also cathode area with relatively negative
specific form or proportion, resulting in a reduction in the rate potential. This non-uniformity will make the surface of the
of corrosion of the material. For steel and iron materials used steel bar more prone to electrochemical corrosion. Especially
in concrete iron materials, the corrosion inhibitor is usually when part of the electrolyte exists on the surface of the steel
defined in the academic field as: when a substance is added bar, it is easy to form a simple electrochemical reaction pool
to make the corrosion rate of the reinforced concrete system on the surface of the steel bar, and each electrochemical reac-
reduced, then this substance is called a corrosion inhibitor tion pool is equivalent to a small galvanic cell on the surface of
the steel bar. Corrosion inhibitors tend to take advantage of
* Corresponding author. naturally existing gaps within the concrete and react chemi-
E-mail address: 2811004@stu.zykj.edu.cn (Y. Wang).
cally at the rebar/concrete interface in the form of a gas or liq-
Peer review under responsibility of Faculty of Engineering, Alexandria
uid phase to the surrounding steel material. It can induce the
University. surface of the rebar to be oxidized to generate a passivation
https://doi.org/10.1016/j.aej.2022.11.020
1110-0168 Ó 2022 THE AUTHORS. Published by Elsevier BV on behalf of Faculty of Engineering, Alexandria University.
This is an open access article under the CC BY-NC-ND license (http://creativecommons.org/licenses/by-nc-nd/4.0/).
Please cite this article in press as: A. Zhang et al., Preparation of inorganic-polymer nano-emulsion inhibitor for corrosion resistance of steel reinforcement for con-
crete, Alexandria Eng. J. (2022), https://doi.org/10.1016/j.aej.2022.11.020
2 A. Zhang et al.

film, or to form a precipitation film with ions in the hole solu- were analytical grade. Carbon nanotubes were purchased from
tion in the cathodic region. Therefore, corrosion inhibitors can Xianfeng Nanotech. Co.
extend the life cycle of the rebar/concrete system [5–9].
The composition of early corrosion inhibitor mainly 2.2. Characterizations
includes various sodium nitrite salts. Nitrite type corrosion
inhibitor is often the most carrier of water-based materials, The electrochemical workstation used is CHI760 from Shang-
which has the advantages of low price, convenient use, good hai C&H Instruments Co. The X-ray diffractometer was an
prevention effect and easy removal [10–14]. Therefore, it con- AXS D8 from Bruker, Germany, and the scanning electron
tinues to be widely used in corrosion inhibitors until today. microscope was a Nova nanoSEM FEI 430 from JEOL,
However, after drying, a layer of white frost often forms on Japan. The infrared spectrometer is Nicolet 6700, USA.
the surface of the workpiece treated with this corrosion inhibi-
tor, which affects the cleanliness of the product. At the same 2.3. Preparation of corrosion inhibitor
time, the formed layer is not stable enough and is prone to flow
and shrinkage, which not only affects the appearance of the
Weigh a certain mass of tap water, inorganic corrosion inhibi-
steel, but also has an impact in the subsequent processing pro-
tor and organic corrosion inhibitor in the beaker. Fix the speed
cess. With the increasing awareness of environmental protec-
of magnetic stirrer to 80 r/min and add water, inorganic corro-
tion, nitrite, which is recognized as a carcinogen, has also
sion inhibitor and organic corrosion inhibitor in turn. For
been subject to some resistance, which also makes the use of
some corrosion inhibitors which are difficult to dissolve, dis-
nitrite-based corrosion inhibitor has been limited in recent
solve them after heating in the constant temperature water
years. Later there was a phosphate (mainly Na2PO3F) based
bath for a certain time and then add them into the magnetic
corrosion inhibitor [15–21]. Phosphates have also received a
stirrer. After adding water, inorganic corrosion inhibitor and
lot of attention because of their remarkable inhibition of chlo-
organic corrosion inhibitor, the stirring was continued for
ride ion attack. However, in actual production, the phosphate
0.5 h, and finally a uniform solution of inhibitor was obtained.
process will have phosphorus discharge, causing serious
Table 1 shows the sample number and contents of the fluoro-
eutrophication of water bodies. At the same time, the phos-
carbon with different contents. 10 % of acrylic resin, VAE-
phate process equipment is more complex and difficult to
707, polyethylene wax, epoxy resin, fluorocarbon nano-
maintain, so it also makes the use of phosphate-based corro-
emulsion DF-1, silicon propylene, pure propylene and benzene
sion inhibitors is limited [22–28].
propylene were also used for preparation of inhibitors and
Water-soluble polymer nano-emulsions, such as acrylic
denoted as sample 4–11.
resin nano-emulsions and fluorocarbon nano-emulsions, have
Before the treatment, the rebar samples were first weighed
a certain viscosity and can exist stably after forming a film
with a balance and then warmed up in a drying oven to the
on the metal surface, which is expected to improve the
lower cooling bed temperature of the rebar for 10 min. The
anti-corrosion performance of steel bars. In this work an envi-
bars were removed from the drying oven and quickly immersed
ronmentally friendly inorganic–organic composite corrosion
in the inhibitor solution for about 2 s. The bars were removed
inhibitor was prepared by adding different kinds of nano-
and dried naturally at room temperature, thus forming a coat-
emulsions using sodium carbonate as the basic raw material.
ing on the surface of the bar samples.
This work analyzed the corrosion inhibition rate of the corro-
The electrochemical workstation and the integrated electro-
sion inhibitor by electrochemical accelerated corrosion test.
chemical test system were used for the dynamic potential
Also, the anticorrosive properties of steel bars treated with
polarization curve test and the electrochemical impedance
corrosion inhibitors under water ambient atmosphere were
spectroscopy test, respectively. A three-electrode system was
investigated. Analysis of the relationship between nano-
used, with the auxiliary electrode (counter electrode) being a
emulsion type, rebar temperature, corrosion inhibitor temper-
platinum electrode, the reference electrode being a saturated
ature and treatment time and corrosion inhibition rate were
glycerol electrode, and the working electrode being a prepared
also investigated. By measuring the XRD diffraction patterns
rebar. The prepared rebar was immersed in the solution to be
of the corrosion products, the SEM images of the rebar before
tested for 30 min. After the open circuit corrosion potential
and after the treatment and the IR spectra of the corrosion
was stabilized, the polarization curves and electrochemical
inhibitor, this work proposed the mechanism of corrosion inhi-
impedance spectroscopy experiments were carried out. The
bitor on the surface of the rebar.
polarization curves of kinetic potential were scanned at a rate
of 0.05 mV/s, and the polarization range was 1. 2 to 0. 5 V
2. Experimental

2.1. Regents

Table 1 Sample number and contents of the fluorocarbon

Sodium carbonate was purchased from Shangyu Jiangfeng
Chemical Co. Fluorocarbon nano-emulsion DF-1 was pur-
chased from Tengfei Plastic Material Co. Rebar was purchased
from Iron City Steel Co. Acrylic resin, VAE-707, polyethylene
wax, epoxy resin, fluorocarbon nano-emulsion DF-1, silicon
propylene, pure propylene and benzene propylene were pur-
chased from Shanghai Wenhua Chemical Co. All chemicals
nano-emulsion with different contents.
Sample number DF-1 (wt.%)
1 40
2 60
3 100

Please cite this article in press as: A. Zhang et al., Preparation of inorganic-polymer nano-emulsion inhibitor for corrosion resistance of steel reinforcement for con-
crete, Alexandria Eng. J. (2022), https://doi.org/10.1016/j.aej.2022.11.020
Preparation of inorganic-polymer nano-emulsion inhibitor for corrosion resistance of steel reinforcement for concrete
(vs OCP). The electrochemical impedance spectroscopy test
was performed in the frequency range of 0. 01 Hz to
100 kHz, with an open circuit potential and an amplitude of
5 mV.
3. Results and discussion
We tested three samples of waterproof test. After 24 h of the
rain, the surface of the three samples has a small amount of
red brown rust, but it is very unknown, and it is shown that
the anti-rust agent formed by this component system has cer-
tain corrosion resistance in 24 h. However, as the erosion time
of the rain erosion increases to 48, the surface of the steel bar
has obvious points and continuous red brown rust. The results
show that the surface of the corrosion resistant layer is washed
by the rain after the long rain erosion test. The rust film is
destroyed by different degrees, which causes the rust of the
reinforcement.
Fig. 1A shows the Tafel curves of the steel bars treated with
different contents of fluorocarbon nano-emulsions. From the
figure, it can be seen that the self-corrosion potential of the
steel bars after treatment with fluorocarbon nano-emulsion is
significantly higher. At the same time, the anodic corrosion
current is significantly reduced, indicating that the fluorocar-
bon nano-emulsion is an anodic inhibitor. The electrochemical
EIS spectrum (Fig. 1B) shows that the impedance spectrum
semicircle radius of steel bars treated with fluorocarbon
nano-emulsion is much larger than that of untreated ones,
which indicates that the impedance of electrons passing
through the electrode surface of steel bars in aqueous solution
is greater and good corrosion resistance can be expected.
Table 2 shows the results of Tafel test analysis of steel bars
treated with fluorocarbon nano-emulsion. It can be seen from
the table that after the fluorocarbon nano-emulsion treatment,
as the content of fluorocarbon nano-emulsion increases from
40 % to 100 %. The self-corrosion potential of the rebar
increased from 0.671 V to 0.592 V, and the polarization
resistance increased from 610.1 X to 1380.8 X. This indicates
that increasing the amount of fluorocarbon nano-emulsion
Fig. 1 (A) Tafel curves and (B) EIS of untreated steel bars and steel bars treated by fluorocarbon nano-emulsion. (B) EIS of untreated
steel bars and steel bars treated by fluorocarbon nano-emulsion.
Please cite this article in press as: A. Zhang et al., Preparation of inorganic-polymer nano-emulsion inhibitor for corrosion resistance of steel reinforcement for con-
crete, Alexandria Eng. J. (2022), https://doi.org/10.1016/j.aej.2022.11.020
3
coating on the surface of the rebar can improve its corrosion
resistance [29,30].
Fig. 2A shows the Tafel curves of steel bars before and after
treatment with inorganic-polymer nano-emulsion compound
inhibitors containing different types of nano-emulsions. From
the figure, it can be seen that the self-corrosion potential of
steel bars after treatment with inorganic-polymer nano-
emulsion compound inhibitors containing different kinds of
nano-emulsions is significantly increased, only the degree of
increase is different. The anodic corrosion current is signifi-
cantly reduced, which is similar to that of inhibitors without
polymer nano-emulsions, indicating that such inorganic-
polymer nano-emulsions belong to the anodic type of inhibi-
tors [31,32]. The electrochemical EIS spectrum (Fig. 2B) shows
that the steel bars were treated with inorganic-polymer nano-
emulsion compound inhibitors containing different types of
inorganic-polymer nano-emulsions. It can be seen that the
half-circle radius of the impedance spectrum is much larger
than that of the untreated one, indicating that the impedance
of electrons passing through the electrode surface of the rebar
in aqueous solution is greater after the rebar is treated with
inhibitors, and the rebar can be expected to have good corro-
sion resistance [33].
This work chose fluorocarbon nano-emulsion DF-1 for the
inorganic-polymer nano-emulsion composite corrosion inhibi-
tor and explored the effect in the presence of 0.01 % carbon
nanotubes. Fig. 3A shows the Tafel curves of steel bars before
and after treatment with inorganic-polymer composite
inhibitor containing different contents of fluorocarbon nano-
emulsion DF-1. It can be seen from the figure that the self-
corrosion potential of the reinforcing steel is significantly
increased and the anodic corrosion current is significantly
reduced after the treatment with inorganic-polymer composite
inhitibor containing different contents of fluorocarbon nano-
emulsion DF-1. The electrochemical EIS spectrum (Fig. 3B)
shows that the radius of the impedance spectrum of steel bars
treated with inorganic-polymer composite inhibitor containing
different levels of fluorocarbon nano-emulsion DF-1 is much
larger than that of untreated bars. This indicates that the impe-
4 A. Zhang et al.

Table 2 Tafel analysis results of untreated steel bars and steel bars treated by fluorocarbon nano-emulsion.
Sample Corrosion potential (V) Rct (X) Corrosion current density (J) Corrosion inhibition rate (%)
Blank 0.671 610.1 8.106 0
1 0.633 1007.4 6.503 18.4
2 0.617 1244.3 5.406 38.1
3 0.592 1380.8 4.995 42.3

Fig. 2 (A) Tafel curves and (B) EIS of untreated steel bars and steel bars treated by the inorganic and polymer nano-emulsion inhibitor
with various nano-emulsion.

Fig. 3 (A) Tafel curves and (B) EIS of untreated steel bars and steel bars treated by the combined inhibitor with the fluorocarbon nano-
emulsion of different contents.

dance of electrons passing through the electrode surface of the
rebar in aqueous solution is greater after the rebar is treated
with such composite inhibitor, and the rebar can be expected
to have good corrosion resistance [34,35].
This work investigated the mechanism of corrosion protec-
tion by analyzing IR spectra. Fig. 4A shows the IR spectra of
inorganic-polymer composite inhibitor and fluorocarbon
nano-emulsion DF-1. It can be seen from the figure that the
IR spectra of the inorganic-polymer composite inhibitor and
the fluorocarbon nano-emulsion DF-1 are similar. The absorp-
tion peaks of the spectrum are located at 3438 cm 1 and
1640 cm 1 are the characteristic absorption peaks of bending

Please cite this article in press as: A. Zhang et al., Preparation of inorganic-polymer nano-emulsion inhibitor for corrosion resistance of steel reinforcement for con-
crete, Alexandria Eng. J. (2022), https://doi.org/10.1016/j.aej.2022.11.020
Preparation of inorganic-polymer nano-emulsion inhibitor for corrosion resistance of steel reinforcement for concrete 5

Fig. 4 (A) IR spectra of the inorganic and macromolecule combined inhibitor and fluocarbon nano-emulsion DF-1. (B) XRD patterns
of corrosion products of the steel bars without inhibitor treatment and treated using inorganic and macromolecule combined inhibitor.

vibration and the characteristic absorption peaks of stretching
vibration of water [35,36]. The infrared absorption peak at
1403 cm 1 is the characteristic absorption peak of CAH bond
stretching vibration, which indicates the presence of –CH2 and
–CH2- groups in the inhibitor. The infrared absorption peak at
1091 cm 1 is a C-F bond stretching vibration peak. The IR
absorption peaks at 630 cm 1 and 474 cm 1 are the C-CO-C
and C–C‚O intra-planar bending vibration peaks [37,38],
respectively.
This work also analyzed the XRD patterns of the corrosion
product on the surface of rebar without inhibitor treatment
and after inorganic-polymer composite inhibitor. As shown
in Fig. 4B, the corrosion product produced by the corrosion
of the rebar mainly consisted of Fe2O3 (JCPDS: 25–1402)
and Fe3O4 (JCPDS: 65–3107), indicating that the singlet iron
on the surface of the rebar produced iron oxide through elec-
trochemical reaction [39]. The crystalline phases of the corro-
sion product on the surface of the rebar without inhibitor
treatment and after inorganic-polymer composite inhibitor
are similar. The above results indicate that the composition
of corrosion products was not changed by the inhibitor after
the treatment of steel bars, and the corrosion products were
mainly composed of Fe2O3 and Fe3O4.
The microscopic morphology of the surface of the
untreated and inorganic-polymer composite inhibitors was
analyzed by scanning electron microscopy, as shown in
Fig. 5. From Fig. 5A and 5B, it can be seen that the surface
of the untreated rebar is smooth and there are micron-sized
grooves on the surface of the rebar. After the inorganic-
polymer composite inhibitor treatment, the surface of the
rebar was covered by a denser inhibitor film layer (Fig. 5C).
According to the theory of thermodynamics, matter seeks to
exist in the lowest energy state, and hydrogen bonding is a
way to reduce chemical energy. Water is a polar substance
and therefore can form hydrogen bonds internally. Because
hydrophobic substances are non-electronically polarized and
cannot form hydrogen bonds, water repels hydrophobic sub-
stances. The hydrophobic effect is caused by the fact that water
itself can form hydrogen bonds with each other. Polymer fluo-
rocarbon nano-emulsions are hydrophobic substances. After
curing on the steel surface, the fluorocarbon nano-emulsion
is compounded with other corrosion inhibitors to form
cross-linked by fluorocarbon polymers and carbon nanotubes.
This dense inhibitor film with hydrophobic effect prevents
water molecules from entering the surface of the rebar and
inhibits the corrosion of the rebar. The untreated rebar is

Fig. 5 SEM images of the steel bars (A) without anti inhibitor treatment and (B,C) treated using inorganic and macromolecule
combined inhibitor.

Please cite this article in press as: A. Zhang et al., Preparation of inorganic-polymer nano-emulsion inhibitor for corrosion resistance of steel reinforcement for con-
crete, Alexandria Eng. J. (2022), https://doi.org/10.1016/j.aej.2022.11.020
6 A. Zhang et al.
not protected by the inhibitor leading to the contact between
the rebar and water. There is a serious electrochemical reaction
of dissolved gold and oxygen absorption on the surface of the
rebar, which makes the rebar have a serious corrosion
phenomenon.
4. Conclusion
In summary, this work prepared an environmentally friendly
inorganic–organic composite inhibitor using sodium carbonate
as the basic raw material and adding different kinds of nano-
emulsions. This work investigated the corrosion inhibition rate
of the antirust agent by electrochemical accelerated corrosion
test and studied the anticorrosion performance of steel bars
treated with inhibitor under water environment. The effect of
nano-emulsion type on the corrosion inhibition rate of rein-
forcing steel shows that different types of nano-emulsions
can improve the self-corrosion potential and reduce the corro-
sion current. The results of the effect of the fluorocarbon nano-
emulsion content on the corrosion inhibition rate showed a
decrease in the content of the fluorocarbon nano-emulsion
DF-1. XRD analysis showed that the corrosion products con-
sisted of Fe2O3 and Fe3O4, and SEM analysis showed that the
surface of the reinforcement was covered by a dense antirust
film after the inorganic-polymer composite antirust agent
treatment.
Declaration of Competing Interest
The authors declare that they have no known competing
financial interests or personal relationships that could have
appeared to influence the work reported in this paper.
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