Cement and Concrete Composites 155 (2025) 105835

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Cement and Concrete Composites

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The corrosion-inhibitory influence of graphene oxide on steel

reinforcement embedded in concrete exposed to a 3.5M NaCl solution
L. Djenaoucine a , C. Argiz a , Á. Picazo b , A. Moragues a , J.C. Gálvez a,*
a
Departamento de Ingeniería Civil: Construcción, E.T.S de Ingenieros de Caminos, Canales y Puertos, Universidad Politécnica de Madrid, c/Profesor Aranguren 3, 28040,
Madrid, Spain
b
Departamento de Tecnología de la Edificación, E.T.S. de Edificación, Universidad Politécnica de Madrid, Avda. Juan de Herrera, 6, 28040, Madrid, Spain

A R T I C L E I N F O A B S T R A C T

Keywords: Steel reinforcement corrosion significantly reduces the durability and service life of concrete structures,
Concrete particularly in chloride-rich environments such as marine and coastal areas. This study aims to reduce the
Graphene oxide corrosion rate using graphene oxide (GO) as a corrosion inhibitor. Two GO dosages (0.0005 and 0.005 wt%) were
Corrosion inhibition
evaluated for their effectiveness in mitigating corrosion in reinforced concrete exposed to a 3.5M NaCl solution.
Reinforcing steel
Chloride environment
To assess the corrosion behavior of the steel reinforcement, Open Circuit Potential (OCP), Electrochemical
Electrochemical measurements Impedance Spectroscopy (EIS), and Linear Polarization Resistance (LPR) were evaluated over one year by
wetting/drying cycles. Oxygen permeability and electrical resistivity tests were also conducted to evaluate the
concrete’s susceptibility to corrosion. Both GO content demonstrated significant corrosion inhibition, with the
0.005 wt% dosage providing the most effective protection. This was evidenced by the lowest icorr values recorded
during the final cycle (52), larger capacitive loops, and higher impedance in EIS results, indicating enhanced
corrosion resistance. Visual inspection of steel bars further confirmed these findings, showing no signs of dete­
rioration or discoloration in GO-modified concrete compared to steel bars extracted from reference concrete.
SEM-EDS analysis revealed higher carbon content on the steel surface, suggesting GO adsorption and the for­
mation of a protective passive layer. These results suggest that GO is a promising nanomaterial for inhibiting
corrosion in steel-reinforced concrete exposed to aggressive environmental conditions.

1. Introduction interconnected pores of concrete and cause crack initiation and propa­
gation [3]. Consequently, when chloride ion concentrations exceed a
Reinforced concrete is a prevalent building material in various en­ critical threshold at the steel surface, they can locally break the passive
gineering fields due to its plentiful and low-cost raw materials. Unfor­ layer formed of iron oxides, hydroxides, and oxyhydroxides, resulting in
tunately, reinforced concrete can be susceptible to durability issues such the formation of voluminous corrosion products that exert internal
as the chemical degradation of the matrix and the corrosion of rein­ stresses and induce fractures in the concrete [4,5]. Numerous factors
forcement in certain environments. The embedded steel bars corrode on affect the rate of steel bar corrosion, such as concrete porosity, chloride
the concrete surface due to carbonization and chloride ion penetration, concentration, oxygen diffusion, concrete strength, etc.
causing cracking and spalling of the concrete cover and strength Thus, substantial scientific research has been devoted to improving
degradation of the steel bar [1]. The corrosion of steel reinforcement in concrete’s durability and service life. In particular, corrosion of steel
concrete is one of the major causes of degradation mechanisms affecting bars. Several approaches have been proposed and implemented to stop
reinforced concrete structures’ durability. The service life reduction of or delay the mechanism of corrosion, such as cathodic protection sys­
concrete structures is a pervasive problem, especially in marine and tems [6], using stainless steel bars [7], coating the steel bars with epoxy
coastal regions with extreme chloride conditions [2]. The penetration of [8–11], and corrosion inhibitors [12–15]. However, many of these
chloride ions into concrete is one of the most significant obstacles to techniques have significant drawbacks. For example, some methods
corrosion resistance and a key factor in shortened service life. Chloride offer insufficient corrosion protection, while others, like using
ions can reach the surface layer of the steel bars through the stainless-steel bars or epoxy coatings, involve very high costs due to

* Corresponding author.
E-mail address: [Link]@[Link] (J.C. Gálvez).

[Link]
Received 24 June 2024; Received in revised form 11 September 2024; Accepted 2 November 2024
Available online 5 November 2024
0958-9465/© 2024 Elsevier Ltd. All rights are reserved, including those for text and data mining, AI training, and similar technologies.
L. Djenaoucine et al. Cement and Concrete Composites 155 (2025) 105835

Fig. 1. Overview of concrete mixtures, specimen preparation, testing methods, and results.

expensive materials and installation procedures. Additionally, certain corrosion resistance of steel bars embedded in concrete by performing
corrosion inhibitors can have negative environmental effects, including various tests, including accelerated corrosion and electrical resistivity
the release of toxic chemicals or pollutants during their production, tests. Ground granular furnace slag (GGBFS) is also used to adjust the
application, or disposal. Nanomaterials, such as carbon nanotubes, new properties of concrete in different proportions (15, 30, 45 wt%).
nano-cellulose, nanoSiO2, nano-TiO2, and graphene oxide (GO), are This study demonstrates that the incorporation of GO to GGBFS en­
considered promising corrosion inhibitors for concrete cover protection hances the compressive strength of the concrete through a synergistic
due to their ability to enhance the concrete microstructure and mechanism. Moreover, the study reveals that the composite with 0.03 wt
concrete-rebar interface area by accelerating the hydration process, % GO exhibits the highest corrosion resistance among all the mixtures,
resulting in concrete with reduced porosity [16,17]. Previous research even in saltwater immersion.
has examined the corrosion resistance of embedded steel reinforcement As discussed in this section, a multitude of studies have focused on
in cementitious materials containing nanomaterials. According to Sal­ the impact of diverse nanomaterials on the corrosion protection of steel
oma et al. [18] concrete containing nano-silica has better corrosion reinforcement. Nonetheless, the influence of GO, has not been exten­
resistance than ordinary Portland cement. The nano-SiO2 reacts with the sively explored within the context of reinforced concrete. However,
Ca(OH)2 in concrete to form secondary calcium silicate hydrate, making numerous studies have been performed to assess the influence of GO on
the concrete chemically stable and structurally dense. This enhances the the strength and durability of cementitious materials owing to their
impermeability of the concrete, reducing the corrosion caused by sulfate distinctive properties. GO is a nano-reinforcement derived from gra­
attack. According to a study conducted by Sadawy et al. [19] it was phene. It boasts a high specific surface area, exceptional mechanical and
observed that the corrosion resistance of reinforcing bars increased with thermal conductivity properties, and a surface rich in active oxygen-
increasing nano-TiO2, up to a weight percentage of 1.5 wt%, as a containing groups [23]. GO is formed by adding oxygen-containing
replacement for cement. The research conducted by Vitharana et al. [20] groups to graphene through a chemical process. These groups include
examined the effect of three different dosages of nano-SiO2 and nano-­ hydroxyl (-OH) and epoxy (-O-) located on the basal plane, while
TiO2 (1 %, 3 %, and 5 % wt%) on the mechanical strength and corrosion carbonyl (C=O) and carboxyl (-COOH) groups are distributed at the
resistance of fly ash-based cement mortars. They reported that the sheet edges. The hydrophilic groups facilitate the dispersion of GO in
incorporation of nanoparticles into cement mortar enhanced the mor­ water. Moreover, they serve as nucleation sites that enhance the kinetics
tar’s corrosion resistance in comparison with control samples, as evi­ of hydration and the formation of hydration products [24]. In addition,
denced by reduced rebar pitting depths and a shortened fracture length. active groups can take part in chemical or physical interactions that may
This enhancement is likely due to the formation of a denser matrix, enhance the interfacial bonding with the target material [25]. Due to
increased the content of C-S-H gel, and a reduced Ca/Si ratio when these attributes, GO has become a prominent research topic over the last
compared with the control mix. In a study conducted by Faizal et al. [21] few years and is employed in various materials, including cementitious
the corrosion potential of steel reinforcement in ultra-high-performance materials. A plethora of research has demonstrated the influence of GO
concrete (UHPC) and UHPC modified with nano clay was evaluated by on the nanoscale properties of cementitious materials. The study by Lin
using half-cell potential (HCP) technique. The results demonstrated that et al. [26] has shown the important role of GO in stimulating the cement
the corrosion activity of steel reinforcement embedded in UHPC with a hydration process, as the oxygen-containing functional groups of GO
5 % addition of nano clay exhibited the lowest corrosion potential serve as adsorption sites for both water and cement components and
readings in comparison with UHPC without the addition. Furthermore, seeding sites for cement hydration products. A study by Pan et al. [27]
it was indicated that an increase in nano clay resulted in a decrease in reported that the carboxylic acid groups formed strong covalent bonds
corrosion potential, thereby delaying the initiation of corrosion. Addi­ with the calcium silicate hydrate (C-S-H) gel and that the specific surface
tionally, the study by Bhojaraju et al. [22] seeks to experimentally area of the C-S-H gel increased. These factors enhanced the mechanical
ascertain the impact of graphene (G) and graphene oxide (GO) on the strength of the cement composite. GO improves the microstructure of

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L. Djenaoucine et al. Cement and Concrete Composites 155 (2025) 105835

Table 1
Chemical composition of CEM I 52,5 R Portland cement obtained by XRF.
Element CaO SiO2 Al2O3 Fe2O3 K2 O MgO Na2O TiO2 P2O5 SO3 LOI

Wt. (%) 61.50 20.50 5.03 3.20 1.05 1.45 0.15 0.25 0.19 3.35 2.39

the cement hydration products, as well as adjusts the crystal size and
Table 2
forms a denser and more compact and homogeneous linkage structure
Chemical composition of GO.
[27–29]. The durability of concrete incorporating GO has been widely
investigated, particularly its resistance to aggressive penetrations such Elements Carbon Oxygen Sulfur Nitrogen Hydrogen Purity
as chloride ions and its permeability to water and gas, which are among Wt. (%) 49–56 51–50 0–2 0–1 0–1 99.9
the factors that induce the corrosion of steel reinforcement. Mohammed
et al. [30] noticed through their study that adding GO to the cement
matrix improves the resistance to aggressive elements’ entry by forming particle size of 0–2 mm, two kinds of gravel with corresponding particle
a strong barrier that reduces the movement of aggressive chemicals. sizes of 4–8 mm and 4–12 mm. Graphene oxide (GO), purchased from
Changjiang et al. [31] also found that adding 0.05 wt% of GO into Graphenea®, pre-dispersed in water at a concentration of 4 g/L was
concrete reduced the chloride depth penetration by 56.8 % compared added in two small doses of 0.0005 % and 0.005 % by weight of cement.
with the reference concrete, and the freezing-thawing loss was also A polycarboxylate-based superplasticizer (PCs), called Sika ViscoCrete-
found to be the smallest with GO. The study by Yihong et al. [32] found 20 HE, was also included to enhance the workability of the concrete.
that adding GO in varying amounts to concrete increased electrical The OPC and GO chemical compositions are detailed in Tables 1 and 2,
resistance and reduced chloride ion diffusion. The optimum amount of respectively.
GO was determined to be 0.03 wt%, and it was found that the im­
provements were likely due to the shrinkage of the pores in the concrete 2.2. Steel rebar preparation
microstructure, resulting in a reduction in conductivity. Devi et al. [33]
revealed, via water permeability test, that the addition of 0.08 wt% GO The chemical composition of the steel bars conforms to the B500SD
in a concrete composite treated for 90 days in a curing room reduced the grade, according to the UNE 36068: 2011 standard [34], was as follows
absorption rate by 90 % compared with the reference concrete. It was (in wt.%): 0.30 % Carbon (C), 0.29 % Silicon (Si), 0.40 % Manganese
stated that the reason for the improvements is related to the fact that GO (Mn), 0.05 % Sulfur (S), 0.05 % Zinc (Zn), and the balance of Iron (Fe) to
behaves as a filler nanomaterial in concrete, filling voids at the nano­ make up 100 %. The cleaning procedure for the corrosion steel bars was
scale level and preventing the absorption of additional water molecules. as follows: An HCl:H2O (1:1) solution containing 3.5 g/L of hexameth­
The existing literature has primarily investigated the influence of GO on ylenetetramine (urotropine) was prepared in a beaker. Each steel rebar
the strength and durability of cement-based materials. However, the was submerged in the solution and subjected to ultrasonic treatment for
effect of GO on the corrosion behavior of steel reinforcement embedded 3 min. Then, the steel rebar was rinsed sequentially with tap and
in cementitious composites has not been explored. The preceding dis­ distilled water and dried. Finally, the steel rebar was wrapped with
cussion highlights the prevailing research focus on safeguarding steel adhesive insulating tape, leaving an exposed area of 7.54 cm2 for
reinforcement in cementitious materials by utilising nanomaterials, chloride penetration (see Fig. 2a). This method was replicated for six
either as an additive for cementitious substances or as a protective steel bars of similar dimensions belonging to three distinct concrete
coating for steel. In contrast, the potential influence of GO in this context types, with two steel samples embedded in two concrete specimens of
has been largely neglected. the same type. The ensuing outcomes presented below are the mean of
This investigation aims to assess the influence of GO on the corrosion two samples of the same type.
resistance of steel reinforcement embedded in concrete. The primary
objective is to evaluate the protective effect of GO in the concrete ma­ 2.3. Specimen preparation
trix, specifically within the concrete cover, and its secondary function in
promoting the formation of a passive layer on the steel surface. Concrete An assessment of the influence of GO on the durability of concrete
specimens will be prepared with two GO dosages, 0.0005 % and 0.005 % was conducted using three different mixes namely HBDGO_0005 and
by weight of cement, alongside a reference specimen with no GO. These HBDGO_005, incorporating 0.0005 % and 0.005 % graphene oxide (GO)
specimens will undergo a series of tests, including gas permeability, additives respectively, while HBDGO_0 served as the control without
electrical resistivity, and electrochemical measurements. Finally, after a GO, as indicated in Table 3. The water-to-cement (w/c) ratio and
year of cyclic immersion and drying in a 3.5M sodium chloride solution, superplasticizer (PCs/c) were held constant at 0.45 and 0.40 %,
the corrosion of the steel bars embedded in the concrete will be analyzed respectively, for all the concrete mixes. The following paragraph details
using scanning electron microscopy coupled with energy-dispersive X- the ingredients’ mixing and how long it takes. At first, 25 % of the total
ray spectroscopy (SEM-EDS). water was taken, and a superplasticizer (PCs) was mixed in and stirred
A flowchart summarizing the experimental procedure is presented in manually for 1 min. Afterward, GO was added and stirred for 2 min. The
Fig. 1. It details the preparation of the concrete mixtures with different water-PCs-GO suspension was then set aside until added to the rest of the
graphene oxide concentrations, the shape of the specimens, and the key mixture. An automatic concrete mixer was used to prepare concrete.
tests conducted to assess their properties, including electrical resistivity, Firstly, the two types of gravel (coarse and fine aggregates) and sand
gas permeability, and electrochemical measurements. This Fig. 1 offers a were mixed for 1 min. Afterward, cement was added and blended with
comprehensive visual summary of the methodology followed in this the pre-mixed materials (gravel and sand) for 25 s. Subsequently, 75 %
study. of the total water was poured into the mixer while it was in a rotating
state. The prepared water-PCs-GO suspension then supplemented the
2. Experimental mixture. To conclude, an extra 30 s was applied to blend the ingredients
well together.
2.1. Materials and mix proportion To quantify gas permeability, cylindrical specimens of dimensions
ø100 × 50 mm³ were employed. Concurrently, cylindrical concrete
The concrete mixes in this study featured Ordinary Portland Cement specimens (ø300 × 150 mm³) were utilized for the evaluation of elec­
(OPC) CEM I 52,5 R, and siliceous aggregates consisting of sand with a trical resistivity. Electrochemical examinations were systematically

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Fig. 2. (a) A schematic diagram of a typical concrete test specimen; (b) a schematic view of the experimental setup used for the electrochemical measurements.

Table 3
Mixture proportion of concrete.
Concrete type Cement (kg/m3) C-Agg (kg/m3) F-Agg (kg/m3) Water (kg/m3) Sand (kg/m3) GOa (wt.%) SP(kg/m3)

HBDGO_0 385 495 349 171.46 974 0 1.54

HBDGO_0005 385 495 349 170.54 974 0.0005 1.54
HBDGO_005 385 495 349 161.84 974 0.005 1.54
a
Relative to cement weight.

executed on cylindrical concrete specimens (ø100 × 110 mm³), with active corrosion, B = 26 mV, and for passive corrosion, B = 52 mV), Rp is
pre-prepared steel bars embedded within the fresh concrete. After a a charge transfer resistance, which is considered equivalent to polari­
period of 24 h, the moulds were carefully detached, and the specimens zation resistance, and A is the area attack in cm2.
underwent a curing process within a standard curing chamber main­ Electrochemical impedance spectroscopy (EIS) tests were then per­
tained at a temperature of 20 ± 2 ◦ C and relative humidity of 98 % for a formed using a signal amplitude of 10− 2 V and a frequency range of 100
duration of 28 days. kHz to 0.01 Hz with 10 points per decade. The measured impedance data
were analyzed by Nova 2.4.1 software to simulate a proper electrical
equivalent circuit.
2.4. Electrochemical measurements in chloride environment
2.5. Electrical resistivity test
Electrochemical measurements were initiated after 28 days of curing
the specimens. The measurements were taken after each cycle; each The electrical resistivity at different ages (2, 7, 28, and 90 days) was
cycle consisted of 5 days of wetting in a 3.5M NaCl solution. This was measured by the direct two-probe technique with the Giatec RCON™
followed by 2 days of drying under laboratory conditions at a controlled device, following the procedure specified by the Spanish standard UNE
temperature of 23 ± 2 ◦ C and relative humidity of 50 ± 5 %. The wet­ 83988–1:2008 [38]. The device applied a variable current with fre­
ting/drying cycles were intended to accelerate the chloride transport. quencies ranging from 1 Hz to 30 kHz and recorded the corresponding
The experiments lasted 52 cycles, equivalent to 365 days. Fig. 2b shows electrical resistance of the specimens. The electrical resistivity of the
a schematic representation of the concrete specimen’s dimensions and concrete was then calculated using Equation (2).
the three-electrode setup system for the electrochemical measurements.
Corrosion behaviour over time was monitored using electrochemical A
ρ = × Rc Equation (2)
techniques, Open circuit potential (OCP), linear polarization resistance L
(LRP) and electrochemical impedance spectroscopy (EIS). A potentio­
Where, ρ is the electrical resistivity in (Ω⋅m), A (m2) is the cross-section
stat/galvanostat with FRA 32 module Autolab PGSTAT 204 from Met­
area of contact of the ends of the concrete specimen, L (m) is the height
rohm, Spain with a Nova 2.4.1 software was used to perform
of the specimen, and RC (Ω) is the concrete resistance.
electrochemical corrosion measurements. The open circuit potential
(OCP) was measured during 300s and the values are referred to a 3 M
KCl Ag/AgCl (Metrohm) reference electrode. The LPR tests were carried 2.6. Oxygen permeability test
out in the potential range of 20 mV to +20 mV versus OCP with a scan
rate of 0.1667 mV/s The polarization resistance Rp values were obtained The oxygen permeability of cylindrical concrete specimens (ø100 ×
from the slope ΔE/ΔI at the OCP. 50 mm3) was measured in accordance with the UNE 83981:2008 stan­
According to UNE-EN 112072 [35] and ASTM G102-23 [36], the dard [39]. The specimens were cured for 28 days in a curing chamber
corrosion current density (Icorr) of the specimen can be calculated using and then subjected to a controlled environment in a closed container
the Stern-Geary constant (B) in Equation (1). (65%–75 % relative humidity and 20 ± 2 ◦ C temperature) for the pur­
/ pose of drying water droplets within the pores and attaining a constant
Icorr = B Equation (1) weight. The method involved applying a specified pressure of oxygen
Rp × A
gas and quantifying the time required for the gas to flow through the
where B is a Stern Geary constant [37], that depends on the cathodic and specimen. The oxygen permeability coefficient K was determined for a
anodic Tafel slopes (bα and bc), in our study, we used B = 26 mV (for given pressure P0 using Equation (3).

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L. Djenaoucine et al. Cement and Concrete Composites 155 (2025) 105835

Fig. 3. Open circuit potential (OCP) versus cycles number.

Fig. 4. Corrosion current density (Icorr) versus cycles number.

( ) 2 . Q . P0 . L . η
K m2 = ( ) Equation (3) mV until cycle 18, indicating a low risk of corrosion. Subsequently, the
A . P2 − P2a
OCP value shifted to a more negative range, reaching a minimum value
Q is the volumetric flow rate, Pa is the atmospheric pressure, L is the of − 394 mV in cycle 27. Despite this potential value signifying a high
specimen thickness, η is the dynamic oxygen viscosity, A is the specimen corrosion risk, it is relatively more positive compared with that of
section, and P is the applied pressure. concrete HBDGO_0005. From this minimum value, the potential evolved
towards more positive values and recovered its initial values of
approximately − 200 mV by cycle 45, corresponding to a low risk of
2.7. Optical microscopy and scanning electron microscopy SEM
corrosion. Considering the displacement of the corrosion potentials of
HBDGO_0005 and HBDGO_005 steels towards more positive potentials,
The reinforced concrete samples were subjected to approximately
GO could be considered an anodic corrosion inhibitor.
one year’s worth of electrochemical measurements, or 52 cycles. Then,
The reference concrete HBDGO_0 initially exhibited an initial po­
they were split by diametral compression, and the steel rebars were
tential comparable to that of HBDGO_0005, with values around − 350
extracted. The rebar surface was initially examined visually and further
mV that remained stable until cycle 17. Subsequent to this cycle, the
by an optical microscope and scanning electron microscope Tescan
potential underwent a precipitous decline towards negative values,
Vega-3 (SEM). The surface was also subjected to elemental and mineral
reaching − 500 mV. Unlike HBDGO_0005 and HBDGO_005, in this case,
analyses with energy-dispersive X-ray spectroscopy (EDS).
there was no change in trend towards positive values, but rather, the
potential remained between − 500 mV and − 600 mV until the end of the
3. Results
cycles. The GO-modified concretes HBDGO_0005 and HBDGO_005
exhibited the least negative (most noble) corrosion potential compared
3.1. Open circuit potential (OCP)
to the reference concrete HBDGO_0, indicating that the rebar remained
in a low-corrosion-risk range of > − 200 mV in the last cycle.
The changes in OCP of steel bars embedded in concrete over time are
HBDGO_005 achieved slightly more positive potentials than
shown in Fig. 3. OCP is not a direct measure of the corrosion rate of steel
HBDGO_0005, which could be explained by the polarization effects
bars, but it can indicate the level of corrosion risk they face in concrete.
caused by restricted oxygen transport [40–43] or by the development of
The horizontal dashed lines in Fig. 3 indicate the corrosion potential
a protective layer on the steel surfaces embedded in the GO-modified
limits (low, medium, high, or severe) based on UNE-EN 112072 stan­
concrete.
dard [35]. The OCP (mV) value presented in this study represents the
The OCP measurements showed a shift towards more positive values
mean of the OCP (mV) measurements obtained from two steel bars.
with the addition of GO, particularly at higher contents. This indicates
The initial OCP values for steel reinforcement in HBDGO_0 reference
improved corrosion resistance over time. The shift towards more posi­
concrete was around − 250 mV, which increased progressively to
tive OCP values suggests that GO acts as an anodic-type inhibitor, which
negative values until cycle 18, reaching the medium corrosion potential
reduces the anodic reaction rate by forming a protective layer on the
zone. After cycle 18, the OCP values further declined to around − 500
steel surface. Anodic inhibitors work by altering the metal’s surface
mV to − 600 mV and remained stable at this level until cycle 52, sug­
properties, reducing its tendency to oxidize. Similar behavior has been
gesting severe corrosion of the steel reinforcement.
observed in other studies, where anodic inhibitors cause a positive po­
On the other hand, the OCP values of steel bars embedded in concrete
tential shift due to forming a stable passive film [44,45]. So, it can be
HBDGO_0005 and HBDGO_005, with 0.0005 % and 0.005 % GO con­
concluded that GO functions effectively as an anodic-type inhibitor,
centrations, respectively, exhibit similar patterns. The initial OCP value
enhancing the corrosion resistance of steel reinforcement in concrete.
of the steel bar in concrete HBDGO_0005 is − 235 mV. This value re­
The corrosion current density (Icorr) of steel bars is a critical factor in
mains within a range of − 250 to − 350 mV, indicating a medium risk of
assessing the corrosion behavior of steel bars in concrete. Fig. 4 shows
corrosion up to cycle 18. Thereafter, the OCP undergoes a negative shift,
the Icorr of the steel bars in HBDGO_0, HBDGO_0005, and HBDGO_005
evidencing an increased risk of corrosion. The minimum OCP value is
specimens as a function of the exposure duration of 52 cycles, equivalent
attained in cycle 32, with a value of − 470 mV. From this point onward,
to one year of cyclic wet-dry conditions. The Icorr of the rebar embedded
the trend reverses, and the potential exhibits a positive shift. By the 42nd
in the reference concrete HBDGO_0 ranged from 0.05 to 0.08 μA/cm2
cycle, the potential reverts to its initial values, approximately − 230 mV,
throughout the initial cycles until the 28th cycle, indicating a negligible
suggesting a return to a medium corrosion risk level. The OCP of the
corrosion zone. However, beyond this point, the Icorr values increased to
steel bar in concrete HBDGO_005 was initially more positive than in
about 0.18 μA/cm2, oscillating from 0.18 to 0.22 μA/cm2 for the
HBDGO_0005, at approximately − 150 mV, and remained around − 200

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Fig. 5. EIS plots (Nyquist and Bode) of steel bars embedded in specimens concrete HBDGO_0, HBDGO_0005, and HBDGO_005, (a-1, a-2) 0 cycle, (b-1, b-2) 28 cycles
and (c-1, c-2) 52 cycles.

remaining cycles which is indicative of low corrosion. For the steel bars gradual increase from 0.01 μA/cm2 to 0.07 μA/cm2, which was the peak
embedded in concrete HBDGO_0005 and HBDGO_005, the Icorr values value, followed by a subsequent decrease from 34 cycles until reached
differ from the reference concrete HBDGO_0. The Icorr of the rebars in the 0.010 μA/cm2 in the final cycle. The addition of GO in the concrete
HBDGO_0005 specimens ranges between 0.07 and 0.17 μA/cm2, i.e., achieves the passivation of the reinforcement at the end of the cycles
between two zones of negligible and low corrosion up to the 36th cycle. with current density values 5 and 10 times below the limit of 0.1 μA/
Thereafter, from this cycle, it declines steadily over the remaining cycles cm2. The incorporation of 0.005 wt% GO (HBDGO_005 concrete)
and reaches a value of 0.02 μA/cm2 in the last cycle. While the Icorr effectively maintains the corrosion current density below 0.1 μA/cm2, a
values of the rebar in HBDGO_005 concrete specimens exhibited a threshold that indicates the retention of the passive state of the

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reinforcements throughout the entire period of exposure to chloride

ions.
As shown in Fig. 4. Icorr initially increases up to approximately cycle
24. This increase can be attributed to the consumption of oxygen trap­
ped in the micro- and nano-pores of the concrete matrix during the fresh
concrete mixing process. Over time, as this initial oxygen supply is
exhausted, an oxygen concentration gradient is established, and oxygen
begins to diffuse through the concrete to reach the steel reinforcement.
Consequently, the amount of oxygen reaching the rebar surface becomes
the controlling factor for the corrosion rate [46–48]. In the GO-modified
concrete, the Icorr value decreases after 24 cycles, which can be explained
by the depletion of the stored oxygen in the matrix and the reduced Fig. 6. Equivalent electrical circuit describing the steel/concrete interface of
diffusion of oxygen from the surrounding environment into the concrete steel bars embedded in concrete specimens HBDGO_0, HBDGO_0005,
matrix modified with GO. This reduction in oxygen diffusion is due to and HBDGO_005.
the beneficial effects of GO, particularly at advanced ages, where it acts
as a filling agent that refines the pores and strengthens the microstruc­ increased the corrosion rate and may have compromised the integrity of
ture, thereby inhibiting further oxygen ingress [25]. Additionally, GO the protective layer at the steel/concrete interface due to higher chloride
serves as a nucleation site (seeding effect) for hydration reactions, concentration and corrosion reactions [37,55].
leading to the formation of additional hydration products that densify Nevertheless, upon reaching cycle 52, both the capacitive loop arc
and compact the concrete matrix [25,49]. GO also promotes continuous radius and the impedance value of steel bars in HBDGO_0005 and
hydration over time; its large surface area and hydrophilic functional HBDGO_005 exhibited a resurgence to a level surpassing that of cycle
groups act as a water reservoir, gradually releasing stored water and 28, whereas those of steel bars in HBDGO_0 persisted in diminishing
providing internal curing during long-term hydration. This ongoing considerably. This phenomenon can be attributed to the emergence of a
hydration process helps develop a dense microstructure that offers barrier film at the steel-concrete interface Furthermore, with regard to
enhanced protection to the embedded steel against corrosion. The the concrete resistance (Rs), the incorporation of GO enhanced the
observed improvement in performance at 52 cycles is consistent with corrosion resistance of steel bars after a certain exposure duration,
previous studies, which show that GO enhances hydration kinetics and which can be elucidated by the enduring influence of GO on hydration
promotes the formation of a compact structure that reduces perme­ kinetics, particularly at later stages. This augmented the hydration de­
ability and corrosion rates [43,50–52]. In contrast, in the reference gree and rendered the cement matrix more compact and homogeneous,
concrete specimen (without GO), oxygen from the surrounding envi­ impeding the diffusion of chloride and oxygen and fostering the refor­
ronment continues to diffuse through the pore network, leading to a mation of the protective layer on the steel reinforcement [43,56,57].
sustained increase in Icorr values for the reinforcing steel. Extended exposure to GO also modifies the steel/concrete interface,
Electrochemical impedance spectroscopy (EIS) is a highly effective creating a more corrosion-resistant layer that reduces the corrosion rate
method for analysing how steel rebars corrode under concrete cover. relative to GO-free concrete.
One of the principal applications of EIS is the study of the electrolyte/ The EIS Nyquist plot may be fitted to an equivalent circuit shown in
electrode interface. Fig. 5 shows the Bode and Nyquist plots of steel bars Fig. 6. This equivalent circuit consists of a parallel circuit connected in
embedded in specimens concrete HBDGO_0, HBDGO_0005, and series with the concrete resistance (RS). The parallel circuit comprises
HBDGO_005 for three cycles of significance: the first and last cycles, the charge transfer resistance of the electrode, (RCT) in our present case
which were considered as the cycles of interest, as well as the 28th cycle, polarization resistance (Rp) has been used at the place of charge transfer
which was identified as a critical point of analysis due to the notable resistance (RCT), and the electrochemical double-layer capacitance (Cdl)
variations that occurred in this cycle according to the previous LRP at the electrode/electrolyte interface. CPE is the constant phase element
measurements. that replaces the double-layer capacitance (Cdl) to compensate for non-
In the Nyquist plot, the difference of the real axis intercept at low and ideal capacitor behaviour.
high frequencies is the charge transfer resistance (Rct), i.e., the diameter The impedance of CPE is given by Equation (4):
of the semicircle. In a system controlled by activation, Rct is equivalent n
ZCPE = Y−0 1 (jω)− Equation (4)
to the polarization resistance (Rp). Thus, the larger the diameter of the
semicircle the higher the resistance, Rp, and hence, the lower the Where: ZCPE = Impedance of the constant phase element.
corrosion rate [53,54]. The capacitive loop diameters and the imped­
ance modulus values at low to medium frequencies for both Y0 = Admittance (S⋅sn);
HBDGO_0005 and HBDGO_005 were larger than those of HBDGO_0 in j = Imaginary unit;
the three selected cycles (1st, 28th, and 52nd), indicating that the steel ω = Angular frequency (rad/s);
bars in HBDGO_0005 and HBDGO_005 had significantly higher corro­ n = Exponent of the CPE.
sion resistance than those in HBDGO_0. Moreover, the resistance
increased with the GO dose, as the HBDGO_005 specimens with 0.005 % The CPE is characterized by Y0, a factor proportional to the double
GO exhibited the highest resistance among all the specimens. The Bode layer capacitance of ideally capacitive electrodes, n, a phase shift that
plots indicate that the phase angle values are relatively higher for the indicates the capacitance deviation from the ideal condition and ranges
steel rebars of HBDGO_0005 and HBDGO_005 concretes at all ages, from 0 to 1, and ω the frequency in radians per second. The CPE behaves
compared to HBDGO_0 concrete. These differences are more significant as a resistor when n= 0, as a capacitor when n = 1, and as an inductance
in cycle 52, which could suggest the influence of GO in protecting the when n = − 1. Table 4 shows the electrochemical parameters obtained
steel surface. from the fitting process. Equation (5) is used to compute the percentage
As shown in Figs. 5 (a-1, b-1, c-1) and (a-2, b-2, c-2), the capacitive of inhibition (GO) efficiency (η%) [58–60].
loop arc radius and the impedance modulus values of all specimens
decreased from cycle 1 to cycle 28, indicating a reduction in corrosion Rp − R*p
η (%) = × 100 Equation (5)
resistance due to the prolonged exposure time in the NaCl solution. The Rp
combined effects of capillary suction and diffusion during wetting and
drying cycles enhanced the transport of oxygen and chloride, which Where Rp represent the polarization resistances with and without GO,

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L. Djenaoucine et al. Cement and Concrete Composites 155 (2025) 105835

Table 4
Fitting data of the equivalent circuit parameters for steel bars in concrete specimens HBDGO_0, HBDGO_0005, and HBDGO_005.
Cycles Specimens Rs (Ω.cm2) Rp (KΩ.cm2) CPE η% χ2
− 5 − 1 − 2 n
Y0.10 (Ω ⋅cm ⋅s ) n

1-cycles HBDGO_0 555.10 52.86 7.33 0.86 – 0.011

HBDGO_0005 642.86 54.96 5.57 0.88 03.82 0.012
HBDGO_005 688.96 122.95 5.75 0.92 57.00 0.019
28-cycles HBDGO_0 667.77 21.66 8.02 0.75 – 0.010
HBDGO_0005 909.13 24.23 7.50 0.84 10.61 0.015
HBDGO_005 1065.13 57.06 6.70 0.87 67.17 0.018
52-cycles HBDGO_0 461.64 17.10 5.10 0.73 – 0.014
HBDGO_0005 1643.10 350.58 3.96 0.82 95.12 0.041
HBDGO_005 1832.50 389.04 4.84 0.88 97.92 0.044

respectively. against corrosive agents.

The concrete resistance Rs of GO-modified concrete (HBDGO_0005 It is worth noting also that the parameters n, Y0, and χ 2 provide
and HBDGO_005) outperformed reference concrete in all three further insights into the corrosion behavior of the GO-modified concrete
mentioned cycles (1, 28, and 52 days). The reference concrete exhibited specimens. The parameter n, which represents the deviation from ideal
a transient increase in Rs from the first to the 28th cycle, followed by a capacitive behavior, remains relatively high for the GO-modified sam­
pronounced decrease at the 52nd cycle, falling below the Rs of the first ples, especially HBDGO_005, across the different cycles. This suggests
cycle. In contrast, HBDGO_0005 and HBDGO_005 concrete demon­ that adding GO contributes to a more homogeneous and stable surface,
strated a continuous increase in Rs. This suggests that GO stimulates the effectively minimizing corrosion sites. Additionally, the admittance
hydration process and enhances concrete durability, even at advanced parameter Y0, which indicates the ease of current flow at the concrete-
ages. steel interface, shows a marked decrease in the GO-modified speci­
The polarization resistance (Rp) of GO-modified concrete samples mens after 52 cycles. This reduction indicates improved barrier prop­
also surpassed the reference sample in all three evaluation cycles (1, 28, erties and reflects the formation of a more compact and less permeable
and 52 days). Notably, the reference sample exhibited a continuous passive layer. This synergy between the physical barrier properties and
decrease in Rp over time, indicating the onset of corrosion acceleration electrochemical stability explains the superior anti-corrosion perfor­
due to the penetration of chloride ions through the concrete cover to the mance observed in specimens modified with GO.
reinforcing steel. In contrast, the GO-modified samples demonstrated a Overall, the higher n values and lower Y0 in GO-modified samples
transient decrease in Rp from cycle 1 to cycle 28. Despite the reduced underline the beneficial effects of GO in enhancing the concrete’s pro­
oxygen permeability though the GO-modified concrete matrix, the ox­ tective properties and effectively mitigating corrosion over time. These
ygen trapped in the matrix since mixing is consumed in the cathodic results align with findings from a study [61], which also reported a
semi-reaction, resulting in a decrease in Rp. However, from cycle 28 to decrease in Y0 values in the presence of GO. According to this paper, this
cycle 52, a significant increase in Rp (60–62 % compared with the first reduction in Y0 is attributed to GO’s ability to form a dense, imperme­
cycle) was observed. This increase can be attributed to the restriction of able barrier that effectively hinders the diffusion of aggressive ions and
oxygen diffusion from the outside by the concrete matrix and the for­ moisture, thereby improving the overall protective performance of the
mation of a more resistant passive layer at the steel/concrete interface coating. The lamellar structure of GO disrupts ion transport pathways
than the initial layer. GO is adsorbed onto the surface of the hardened and increases resistance against corrosion, resulting in lower capaci­
steel, forming a more protective passive layer that acts as a barrier tance and enhanced coating durability.

Fig. 7. Electrical resistivity evolution in concrete specimens at different curing ages.

8
L. Djenaoucine et al. Cement and Concrete Composites 155 (2025) 105835

Fig. 8. Gas permeability of concretes.

Moreover, the low χ 2 values throughout all cycles confirm that the 3.3. Oxygen (O2) permeability
equivalent circuit model used provides a reliable fit for the experimental
data, supporting the validity of these findings. While the χ 2 values are Assessing oxygen (O2) permeability in concrete samples is important
small and the current circuit model fits the data adequately, we have because oxygen plays a crucial role in steel corrosion within concrete.
observed a slight increase in error over time, particularly up to cycle 52 Reducing O2 permeability makes the cathodic reaction more difficult
in the samples containing GO. This small increase does not significantly [65,66], which inhibits corrosion. Fig. 8 shows the O2 permeability
impact the validity of the current model; however, it may indicate po­ coefficients for all the concrete specimens, each averaged over three
tential modifications in the electrochemical behavior of the system over identical specimens. Notably, adding GO to concrete significantly de­
the long term. creases the O2 permeability coefficient. Compared with the control
concrete (HBDGO_0), the GO-modified concrete types HBDGO_0005 and
3.2. Electrical resistivity HBDGO_005 show a remarkable reduction in O2 permeability co­
efficients of 88.57 % and 95.11 %, respectively.
The durability of concrete depends largely on the properties of its The O2 permeability of concrete is a paramount microstructural
microstructure such as the connectivity between the pores of the ma­ property that reflects the structure and volume of pores [67,68]. The
terial. A finer porous microstructure, with lower connectivity, leads to notably reduced oxygen permeability coefficient of specimens
lower permeability and may be linked to a reduced ingress of aggressive HBDGO_0005 and HBDGO_005 compared with the reference concrete
agents. Electrical resistivity is inversely related to corrosion rates of HBDGO_0 indicates a significant obstruction of most of their pores.
metal reinforcements in concrete [62]. The study evaluated the elec­ According to previous studies [27,69,70], the incorporation of GO into
trical resistivity properties of concrete specimens (without steel bars) at cement composites has been shown to enhance their permeability. GO
different curing ages of 28, 60, and 90 days, with two distinct concen­ plays a crucial role in improving the microstructure of the cement matrix
trations of GO (0.0005 % and 0.005 %) designated HBDGO_0005 and by effectively occupying the pores and voids, thereby enhancing its
HBDGO_005, respectively. Fig. 7 illustrates the outcomes. Compared density and homogeneity. This phenomenon can be attributed to the
with the reference specimen HBDGO_0, specimen HBDGO_0005 high surface area and adsorption capabilities of GO, which effectively
exhibited a 2.90 %, 4.02 %, and 3.17 % increase in electrical resistivity facilitate cement hydration and reduce the porosity of the composite
at 28, 60, and 90 days, respectively. While specimen HBDGO_005 material. Furthermore, incorporating GO into cementitious composites
showed a more pronounced improvement in electrical resistivity of 3.53 provides additional nucleation sites for the precipitation of calcium
%, 5.42 %, and 6.73 % at 28, 60, and 90 days, respectively. According to silicate hydrate (C-S-H) gel, the primary constituent contributing to the
previous research [27,63,64], the superior efficiency of GO in acting as refinement of the pore structure and microstructure. This process ulti­
nucleating sites accelerates cement hydration and subsequently raises mately culminates in a reduction in concrete permeability.
electrical resistivity.
The electrical resistivity measurements corroborate the concrete
3.4. Visual and optical microscopic examination
resistance Rs derived from electrochemical techniques, thus validating
that the incorporation of GO augments the concrete cover resistance.
The optical microscopy analysis of the iron specimens extracted from
This empirical finding implies a reduction in the porosity and pore
the concrete samples after one year of exposure to a 3.5M NaCl solution
connectivity of the GO-modified concrete matrix. Consequently, this
under cyclic wetting and drying conditions is presented in Fig. 9. In
diminished porosity and pore connectivity hinders the penetration of
particular, the steel bar specimen embedded within the reference con­
air, water, or chloride ions into the concrete matrix, thereby resulting in
crete specimen evinces conspicuous blemishes in the form of brown rust
a lower corrosion rate observed in GO-modified specimens, as previ­
spots, distributed across its surface (Fig. 9a). Furthermore, discernible
ously reported.
white spots and deposits are evident, indicative of the diffusion of
chloride ions through the concrete pores and their accumulation on the

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L. Djenaoucine et al. Cement and Concrete Composites 155 (2025) 105835

Fig. 9. Optical micrographs of steel reinforcement extracted from chloride-contaminated concrete (a) HBDGO_0, (b) HBDGO_0005, and (c) HBDGO_005.

steel bar. On the other hand, the GO-modified concrete specimens cycles, there is a significant reduction of the corrosion rate and an in­
exhibit remarkable corrosion protection performance, as evidenced by crease of the polarization resistance of the steel bars embedded in the
the intact and clean appearance of the steel bar surface, with no signs of GO-modified concrete specimens. Therefore, these findings confirm the
deterioration or discoloration (Fig. 9 b and c). These observations are in effectiveness of GO as a corrosion inhibitor for steel reinforcement in
agreement with the findings derived from the electrochemical mea­ concrete.
surements technique employed to monitor the corrosion dynamics of
steel reinforcement within concrete, as mentioned above, at the last

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L. Djenaoucine et al. Cement and Concrete Composites 155 (2025) 105835

Fig. 10. SEM-EDS characterization of rebar surface that was embedded in (a) HBDGO_0; (b) HBDGO_0005; and (c) HBDGO_005.

3.5. Scanning electron microscopy - energy dispersive X-ray spectroscopy images of the steel bar surfaces, while Table 4 summarizes the quanti­
(SEM-EDS) tative results of the EDS analysis. Based on the EDS results, the elemental
iron (Fe) content on the surfaces of the steel reinforcement bar in
The microstructural morphology and elemental composition of the specimen HBDGO_0 was determined to be 49.77 %. This finding in­
steel bars were investigated by SEM-EDS. Fig. 10 displays the SEM dicates that a corrosion reaction has occurred on the steel reinforcement

11
L. Djenaoucine et al. Cement and Concrete Composites 155 (2025) 105835

Fig. 11. Evolution of (a) concrete resistance (Rs); and (b) Polarization resistance (Rp).

bar embedded in HBDGO_0. This was corroborated by a visual exami­ interact with cementitious materials through physical adsorption,
nation of the condition of the steel bar, as shown above in Fig. 9 a. A resulting in a denser microstructure.
quantity of corrosion products was present on the surface of the steel
reinforcement bar, corroborating the results of the EDS analysis. More­ 4. Discussion
over, the elemental Fe content values observed on the surfaces of
specimens HBDGO_0005 and HBDGO_005 were quantified to be 69.67 This scholarly inquiry scrutinizes the potency of Graphene Oxide
% and 72.31 %, respectively. These values were found to be markedly (GO) as a corrosion inhibitor for reinforced concrete structures. The
higher in comparison with the Fe content in HBDGO_0. This substantial evaluation is bifurcated into two integral aspects: (1) the enhancement
discrepancy provides compelling evidence that the incorporation of GO of the concrete matrix’s durability attributed to GO’s heightened resis­
has resulted in the efficacious inhibition of oxidative dissolution of the tance against the permeation of gases and chloride ions; and (2) the
iron. impact of GO on the passive film enveloping the steel surface, as sub­
Additionally, quantitative analysis of the elemental carbon (C) con­ stantiated by SEM-EDS results.
tent on the surfaces of steel bars embedded in HBDGO_0005 and The incorporation of GO into concrete significantly amplifies its
HBDGO_005, as shown in Table 4, revealed significant percentages of resistance (Rs) at advanced stages, thereby safeguarding the structural
approximately 10.85 % and 17.06 %, respectively. On the other hand, integrity of the embedded steel and attenuating the corrosion process.
the steel bars embedded in HBDGO_0 exhibited a substantially lower This is substantiated in Fig. 11a, which illustrates that the Rs values of
estimated C content of merely 1.88 %. Indeed, the composition of GO-modified concrete are markedly higher at later stages (particularly
reinforcing steel includes C, albeit in a low percentage, as confirmed by from the 24th cycle onwards) compared with the reference specimen.
the reference sample. Nevertheless, the C detected in the rebar Moreover, the measurements of electrical resistivity and the oxygen
embedded in the GO-modified sample is unequivocally attributable to permeability coefficient, as depicted in Figs. 7 and 8, respectively,
the GO incorporated on the steel surface, which led to forms a carbon- corroborate the Rs findings. The GO-modified concrete specimens
based protective layer, that acts as a barrier against corrosive agents. manifested a considerable reduction in the oxygen permeability coeffi­
Notably, GO, as shown in Tables 2, is composed of two basic elements: cient, concomitant with an enhancement in electrical resistivity. This
oxygen and carbon. Hence, this observation elucidates the rationale for indicates a diminished rate of total porosity and connective pores rela­
the substantial increase in the polarization resistance (Rp) in the steel tive to the HBDGO_0 reference concrete. According to recent studies [50,
reinforcement embedded in HBDGO_0005 and HBDGO_005 relative to 72], GO exhibits a high specific surface area and is characterized by
the reference sample HBDGO_0, that is, as indicated in Table 3 above, hydrophilic functional groups. These properties enable GO to function as
the polarization resistance in these samples reaches 389.04 kΩ cm2 in a water reservoir when incorporated into a cement matrix. It absorbs the
HBDGO_005 specimen, and 350.58 kΩ cm2 in HBDGO_0005 specimen, surplus water present in the cement paste, thereby mitigating the rapid
whereas 17.10 kΩ cm2 in HBDGO_0 specimen at the end of the 52 cycles. loss of water. As the hydration process ensues, the system may encounter
The chloride content on the surface of the reinforcing steel is another a deficiency of water to maintain the progression of this process. In such
significant parameter, as revealed by the spectra shown in Fig. 10. The instances, the water retained on the surface of the GO is incrementally
rebar embedded in HBDGO_0 exhibits a chloride content of 14.16 %. released. This mechanism ensures the perpetuation of the hydration
whereas both rebar samples embedded in GO-modified concrete show process and facilitates internal preservation, even over an extended
no traces of chloride. This observation serves as empirical evidence of period.
the beneficial impact of GO on the concrete matrix. An increase in Rs is This explains the reduction of Icorr, especially in the final cycles, due
observed in the HBDGO_0005 and HBDGO_005 concretes compared to to the internal curing mechanism of GO after long-term hydration.
the reference concrete, especially from cycle 28 onwards. This increase Nevertheless, the initial increase in the Icorr in the first cycles is
enhances resistivity, and oxygen permeability, and confirms that the attributed to the consumption of available oxygen within the concrete
addition of GO also hinders the diffusion of chloride ions towards the matrix, which is present in the fresh concrete during the mixing process.
steel surface. The paper [71] proposes that the mechanism underlying As well as, starting from cycle 28, there is no proportional correlation
the inhibition of chloride penetration by GO addition is the refinement between the increase in concrete resistance (Rs) and the polarization
of the pore structure through the filling of capillary pores. GO is a resistance (Rp). Therefore, it is inferred that the decrease in the corrosion
nanomaterial with a sheet-like layered structure and a large aspect ratio. rate is not only attributed to the reduction in the permeability of the
It also has various reactive oxygen functional groups that enable it to concrete but also to the formation of a more resistant passive layer on

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L. Djenaoucine et al. Cement and Concrete Composites 155 (2025) 105835

Table 5 Declaration of competing interest

Summary of parameters, abbreviations, and definitions used in the study.
Abbreviations Description Unit The authors declare that they have no known competing financial
2 interests or personal relationships that could have appeared to influence
Icorr Corrosion current density μA/cm
B Stern-Geary Constant mV the work reported in this paper.
OCP Open circuit potential mV
Rs Concrete resistance Ω⋅cm2 Acknowledgments
Rp Polarization resistance kΩ⋅cm2
K Water permeability coefficient m2
Р Electrical resistivity Ω⋅m
The authors gratefully acknowledge the financial support provided
A Cross-sectional area of the specimen in contact with m2 by the Ministry of Economy, Industry and Competitiveness of Spain by
the electrodes means of the Research Fund Project PID2019-108978RB-C31 and
L The height of the specimen m TED2021-130734B-I00.
SEM Scanning Electron Microscopy /
EDS Energy Dispersive X-ray Spectroscopy /
ZCPE Impedance of the constant phase element Ω− 1⋅cm2⋅sn Data availability
Y0 Admittance (S⋅sn)
j Imaginary unit / Data will be made available on request.
ω Angular frequency (rad/s)
n Exponent of the CPE (0 ≤n ≤ 1) /
η inhibition efficiency %
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