CLAY-04035; No of Pages 10

Applied Clay Science xxx (2016) xxx–xxx

Contents lists available at ScienceDirect

Applied Clay Science

journal homepage: www.elsevier.com/locate/clay

Research paper

A novel geopolymer application: Coatings to protect reinforced concrete

against corrosion
Ana María Aguirre-Guerrero ⁎, Rafael Andrés Robayo-Salazar, Ruby Mejía de Gutiérrez
Composites Materials Group (CENM), School of Materials Engineering, Calle 13 # 100-00, Edif. 349. 2° piso, Universidad del Valle, Cali, Colombia

a r t i c l e i n f o a b s t r a c t

Article history: This study evaluates the performance of two hybrid type geopolymer mortars composed of alkaline-activated fly
Received 12 September 2016 ash (FA) and metakaolin (MK) as protective coatings against chloride-induced corrosion in reinforced concrete.
Received in revised form 6 October 2016 In both cases, the coated, Portland cement (OPC)-based concretes (substrates) were subjected to accelerated
Accepted 17 October 2016
techniques such as impressed voltage and wetting/drying (w/d) cycles in the presence of a 3.5% NaCl solution.
Available online xxxx
The corrosion was also monitored by applying techniques involving linear polarization resistance and open cir-
Keywords:
cuit potential. The results allowed for the conclusion that the MK-based geopolymer coating exhibited the best
Concrete performance, reducing the corrosion rate compared to concrete without coating (reference) by 4 cycles of w/d.
Geopolymer After cycle 5, the corrosion rate was similar for the specimens with or without coating. The application of
Coating geopolymer type coatings (mortars) is suggested as a method of protecting structures exposed to marine
Corrosion environments.
Fly ash © 2016 Elsevier B.V. All rights reserved.
Metakaolin

1. Introduction
The corrosion of reinforcing steel is one of the primary mechanisms
of deterioration of reinforced concrete exposed to environments that
contain primarily chloride ions and/or carbon dioxide (Ahmad, 2003).
Chloride attack is one of the most aggressive causes of reinforcement
corrosion; in this case, chloride ions diffuse through the concrete until
they reach the steel, where they accumulate until they reach a critical
concentration that has the capacity to destroy the passive layer of the
steel and initiate corrosion (Angst et al., 2009). When the corrosive pro-
cess is activated, corrosion products are formed that expand in volume,
producing cracking, resistance loss, concrete delamination and structur-
al collapse (Bertolini et al., 2004; Shi et al., 2012).
Preventing the corrosion of reinforcements begins at the design
phase, which must account for structural calculations, material selec-
tion, concrete mix design, and adequate compaction and curing
(Aguirre and Gutiérrez, 2013). However, in spite of these consider-
ations, complimentary methods are necessary to extend the lifetime of
structures, such as the application of coatings, the use of pozzolanic ad-
ditives and electrochemical techniques, and other approaches (Bertolini
et al., 2004).
⁎ Corresponding author.
E-mail addresses: ana.aguirre@correounivalle.edu.co (A.M. Aguirre-Guerrero),
rafael.robayo@correounivalle.edu.co (R.A. Robayo-Salazar),
ruby.mejia@correounivalle.edu.co (R.M. de Gutiérrez).
Among the preventative methods, coatings have been widely used
due to their economic cost-effectiveness and their ability to be applied
directly to rebar or to concrete surfaces, depending on the case. There
are three types of coatings: metallic, organic and inorganic.
Organic and inorganic coatings are the most widely used on concrete
surfaces due to their ease of application, flexibility and adhesion proper-
ties (Brenna et al., 2013; Criado et al., 2015; Criado et al., 2014; Keßler et
al., 2015; Pour-Ali et al., 2015; Saravanan et al., 2007; Selvaraj et al.,
2009). The different types of coatings in this category include paints,
acrylic dispersions, polyurethanes, epoxy resins and waterproof coat-
ings among others (Al-Zahrani et al., 2002; Almusallam et al., 2003;
Batis and Pantazopoulou, 2000; Christodoulou et al., 2013; de Vries
and Polder, 1997; Medeiros and Helene, 2009; Pacheco-Torgal and
Jalali, 2009; Sadati et al., 2015; Swamy and Tanikawa, 1993; Tittarelli
and Moriconi, 2008; Vaidya and Allouche, 2010; Zhu et al., 2013). One
disadvantage of these common coatings (organic and inorganic) is the
progressive loss of their protective action (durability); this is mainly be-
cause their useful lifetime is compromised by aggressive environmental
factors, which makes it necessary to constantly monitor the coatings
and, in most cases, conduct periodic repair work. Recent studies by
Zhang et al., (2010a, b) have proposed the application of geopolymer
coatings as a viable alternative to common coatings to mitigate their du-
rability disadvantages. These authors suggested that geopolymer coat-
ings may be used to protect marine structures given that geopolymers
generally have low permeability and excellent adhesion and anticorro-
sive properties.

http://dx.doi.org/10.1016/j.clay.2016.10.029
0169-1317/© 2016 Elsevier B.V. All rights reserved.

Please cite this article as: Aguirre-Guerrero, A.M., et al., A novel geopolymer application: Coatings to protect reinforced concrete against corrosion,
Appl. Clay Sci. (2016), http://dx.doi.org/10.1016/j.clay.2016.10.029
2 A.M. Aguirre-Guerrero et al. / Applied Clay Science xxx (2016) xxx–xxx
Fig. 1. Schematic of experimental methodology.
Geopolymers, which are also known as alkaline cements or inorgan-
ic polymers, are materials with a tri-dimensional aluminosilicate struc-
ture that result from the chemical interaction between a strongly
alkaline solution and a source of aluminosilicates (Komnitsas and
Zaharaki, 2007; Shi et al., 2011). Although recently it was recognized
that Kulh filed a patent on alkali cements as an alternative to Portland
cement in 1908 (Pacheco-Torgal, 2015), the properties of these type of
cements have been studied since 1930. The results obtained have
shown that they have excellent mechanical properties, a high resistance
to chemical attack and strong fire resistance (Davidovits, 2002; Duan et
al., 2016; Kong and Sanjayan, 2010; Pacheco-Torgal et al., 2008a;
Zhuang et al., 2016). Metakaolin (MK), fly ash (FA) and ground granu-
lated blast-furnace slag (GGBFS) are commonly used as aluminosilicate
sources (Shi et al., 2011).
Metakaolin (MK) is a manufactured pozzolan produced by thermal
processing of purified kaolinitic clay at a temperature of 600 °C to
700 °C. During the calcination process, the chemical bound water in
the interstices of kaolinite is driven off, and the crystalline structure is
destroyed by this reason this material is an amorphous aluminosilicate.
Fly ash (FA) is a solid waste obtained by electrostatic or mechanical pre-
cipitation from the flue gases of furnaces fired with coal. More than 500
million tons of fly ashes are generated each year by power stations, but
the average utilization level is only about 30%, mainly in the cement and
concrete industry as a supplementary cementitious material. In Colom-
bia approximately 600 kt/y of low quality FA which is mainly disposes in
landfills (Mejía et al., 2015) is generated. MK compared with fly ash has
higher purity, finer particle size and higher activity. Field performance
and laboratory research of concrete containing MK have demonstrated
its value as an effective pozzolan in the formulation of high performance
concrete (Aguirre and Gutiérrez, 2013). MK is considered to be a suit-
able precursor for geopolymer production due to its high reactivity
and properties. Zhang et al. (2010a) developed a coating to protect ma-
rine structures based on a binary type geopolymer (90%MK-10%GGBFS)
reinforced with short polypropylene fibres that were incorporated to
mitigate cracking due to shrinkage during hardening. The results
showed that the low permeability, high adhesion and excellent anticor-
rosive properties provided by the coating confirm its suitability as a pro-
tective barrier for marine structures. In a later study, Zhang et al.
(2010b) attributed the protective performance of the geopolymer coat-
ing to its low permeability resulting from its high meso-porosity (22.3%
of total porosity and 94% of pores ≤20 nm) compared to a Portland ce-
ment paste (OPC) (29.5% total porosity and 73.7% of pores ≥50 nm). In
Please cite this article as: Aguirre-Guerrero, A.M., et al., A novel geopolymer application: Coatings to protect reinforced concrete against corrosion,
Appl. Clay Sci. (2016), http://dx.doi.org/10.1016/j.clay.2016.10.029
addition, Zhang et al. (2010b) observed that the geopolymerization
products were stable when immersed in seawater or exposed to air.
These results confirm that geopolymer consisting of 90% MK and 10%
GGBFS can be used as coatings for marine structures.
Another alternative for the use of geopolymer coatings is their direct
application to reinforcing steel. Kriven et al. (2009) applied an MK-
based geopolymer coating to reinforcing bars placed in Portland cement
mortars, which were then subjected to accelerated corrosion tests and
exposed to NaCl at 3.5%. The results showed that the geopolymer coat-
ing improved the resistance to corrosion of the steel embedded in the
mortar. Similarly, Rostami et al. (2015) applied a coating based on the
alkaline activation of FA on reinforcing steel in concrete and found
that the coating significantly reduced the corrosion rate of the reinforc-
ing steel. On the other hand, Temuujin et al. (2009) applied an MK-
based geopolymer coating to metal substrates, which stated that the ad-
hesion properties depend on its chemical composition and showed an-
other application as thermal barriers.
The purpose of this study is to evaluate the potential of two MK- and
FA-based geopolymers as coatings applied to the surface of reinforced
concrete exposed to an artificial marine environment. The corrosive
process was evaluated using accelerated techniques, such as impressed
voltage and wetting/drying (w/d) cycles. The monitoring process was
done through non-destructive techniques, such as open circuit potential
(OCP) and linear polarization resistance (LPR). In addition, scanning
electron microscopy was used to observe the microstructure.
2. Experimental procedure
The methodology carried out in this study is summarized in the
schematic shown in Fig. 1.
2.1. Production of the reinforced concrete (substrate)
To produce the concrete specimens (substrates), the raw materials
available in the national market were selected, including general use
Portland cement, reinforcing steel and natural aggregates (sand and
gravel). A water/cement ratio of 0.55 was used in the production of
the concrete. Table 1 shows the designed concrete mix dosage based
on the procedure in ACI 211 (ACI Method: Mix design of Concrete).
After mixing, the fresh concrete was poured into metallic forms measur-
ing 76.2 × 152.4 mm and compacted with a smooth metallic bar. The
forms were removed from the specimens after 24 h, at which time cur-
ing began underwater for a period of 28 days. The compressive strength
of concrete is presented in Table 1. Each specimen had an embedded
structural steel bar in the centre measuring 150 mm in length and
6.4 mm in diameter (Fig. 3a).
These bars were previously subjected to cleaning with acetone to
eliminate any possible presence of surface grease. In addition, an expo-
sure area of 60 mm in length was marked, which corresponded to the
area embedded inside the concrete. The portion of the bar exposed to
the air was coated with corrosion-resistant epoxy paint.
2.1.1. Obtaining the geopolymer coatings
Table 2 shows the chemical compositions and particle sizes, which
were obtained through X-ray fluorescence (XRF) using a MagiX-Pro
PW–2440 Phillips spectrometer, equipped with a Rhodium tube and
Table 1
Concrete mixes composition and compressive strength of concrete.
Material kg/m3
Cement 389
Water 214
Coarse aggregate 900
Sand 900
Compressive strength at 28 days of curing (MPa) 25
 A.M. Aguirre-Guerrero et al. / Applied Clay Science xxx (2016) xxx–xxx 3

Table 2
Oxide composition and physical properties of raw materials used.

Precursor

MK FA

SiO2 52,36 63,10

Al2O3 44,25 24,41
CaO – 0,97
Fe2O3 0,37 5,66
Chemical composition (weight %) MgO – 0,62
TiO2 1,76 1,31
K2O – 1,79
Other 0,92 1,75
LOIa 0,86 14,6
Physical properties Particle size (μm) 6,57 19,00
a
LOI: Loss of ignition at 1000 °C.

with a maximum power of 4 kW and laser granulometry performed by a

Mastersizer-2000 laser granulometer from Malvern Instruments with a
Hydro2000MU dispersion unit, and distilled water was used as the dis-
persing medium, respectively. The materials used were Metamax®
brand commercial Metakaolin (MK) produced by the company BASF,
fly ash (FA) obtained as a by-product of a Colombian thermoelectric
plant, and general use Portland cement (PC), type I. Fig. 2 shows the
X-ray diffraction pattern obtained for FA and MK, which were obtained
using a PanAnalytical X'Pert-MRD X-ray diffractometer with Cuα radia-
tion and a step size of 0.020 for a 2θ range between 10 and 60°. MK has a
higher amorphous phase compared to FA, which leads to a higher
reactivity.
To improve the stability of the coatings and minimize cracking due
to shrinkage during hardening, river sand and commercial polypropyl-
ene fibres made by Sika (PP) were used. The activating solutions were
formulated using a commercial potassium silicon mixture (26.4% SiO2
by weight, 13.1% K2O by weight, and 60.6% H2O by weight) and 55%
KOH by weight for the FA-based coating or 11.7% for the MK-based coat-
ing. To achieve adhesion to the substrate (in this case, to concrete) and
to avoid thermal curing, 10% Portland cement (OPC) by weight with re-
spect to the precursor was added to the mix (Mejía et al., 2015).
Fig. 3. (a) Reinforced concrete without coating. (b) Reinforced concrete with MK/10OPC
coating. (c) Reinforced concrete with FA/10OPC coating.
The mixtures for the coatings composed of 90% MK and 10% OPC
(MK/10OPC) were formulated (activator + solid precursor) using
molar ratios for SiO2/Al2O3 of 2.8, K2O/SiO2 of 0.28 and H2O/K2O of
10.0 and a liquid/solid ratio (l/s) of 0.4. The mixtures for the coatings
composed of 90% FA and 10% OPC (FA/10OPC) were formulated with
molar ratios for SiO2/Al2O3 of 6.0, K2O/SiO2 of 0.20 and H2O/K2O of
11.0 and an l/s ratio of 0.3. The molar ratios used in this study were ob-
tained from previous research (Mejía et al., 2015; Villaquirán-Caicedo et
al., 2015).
The coatings were made using a cementitious paste with a sand ratio
of 1:2 and incorporating 0.5% PP fibres by volume. Siliceous sand with a
fineness modulus of 1.85 was extracted from a river in the region and
used as a particulate reinforcement. To mechanically characterize the
coatings (compressive strength), 20 mm cubes (mortars) were formed
and cured at room temperature with a relative humidity of approxi-
mately 90%. The cubes were then tested at ages of 3, 7 and 28 days in
an INSTRON universal testing machine at a testing velocity of 1 mm/
min.

2.2. Application of the geopolymer coatings

The application of the coatings was done manually. First, the con-
crete surface was moistened with clean water to saturate the pores
and control unwanted absorption of the water in the coating mixture,

Fig. 2. X-ray diffractogram of FA and MK used. Fig. 4. Compressive strength of coatings after 3, 7 and 28 days of curing (25 °C).

Please cite this article as: Aguirre-Guerrero, A.M., et al., A novel geopolymer application: Coatings to protect reinforced concrete against corrosion,
Appl. Clay Sci. (2016), http://dx.doi.org/10.1016/j.clay.2016.10.029
4 A.M. Aguirre-Guerrero et al. / Applied Clay Science xxx (2016) xxx–xxx

Fig. 5. Macroscopic observation of the substrate-coating interface. (a) Concrete coated with FA/10OPC. (b) Concrete coated with MK/10OPC.

which would affect the workability and correct application. Subse- coated concrete, the coated face was exposed to 3.5% NaCl in the testing
quently, the coatings were mixed so that they could be applied. The cell. The permeability test was done 7 days after the coatings were
coatings were then distributed on the surface of the concrete with a applied.
trowel, taking care to ensure a homogeneous thickness on the specimen
(Fig. 3). 2.4.2. Exposure to chlorides

2.3. Evaluation of substrate-coating adhesion
The adhesion strength was determined using an Elcometer 106 ad-
hesion tester for concrete test specimens measuring 14.5 × 9.6 cm for
both types of coatings (MK/10OPC and FA/10OPC). The test was done
in accordance with ASTM Standard D4541 (Standard Test Method for
Pull-Off Strength of Coatings Using Portable Adhesion Testers). The dolly
was fixed to the coating surface using epoxy adhesive, and the time
and temperature of adhesion were 24 h and 25 °C, respectively. To visu-
alize the concrete-coating interface, a Nikon SMZ 1000 stereomicro-
scope was used at 4.5× magnification.
2.4. Evaluation of the geopolymer coating performance
2.4.1. Permeability to chloride ions
Measurements of the resistance to chloride ion penetration were ob-
tained in accordance with the ASTM Standard C1202 (Standard Test
Method for Compressive Strength of Cylindrical Concrete Specimens); the
PROOVE'it apparatus by German Instruments was used. For comparison,
OPC concrete specimens with and without coating were used. For the
2.4.2.1. Wetting/drying cycles (w/d). The reinforced concrete specimens
with and without coatings were exposed to chlorides (Fig. 3) by
means of w/d cycles (15 days exposed to ambient temperature and sub-
sequently immersed in 3.5% aqueous NaCl solution for 15 days). At the
end of each cycle, open circuit potential (OCP) and linear polarization
resistance (LPR) measurements were performed. Monitoring continued
until cycle 10 was reached. This test was done 7 days after the coatings
were applied.
2.4.2.2. Impressed voltage. The impressed voltage test was done 7 days
after the coatings were applied on the reinforced concrete specimens
in accordance with the Standard NTC BUILD 356 (NordTest Method –
Concrete, repairing materials and protective coating: Embedded Steel
method, chloride permeability). The objective of the test was to verify
the vulnerability to corrosion of the steel embedded in concrete with
and without coatings in the presence of chlorides. To that end, the spec-
imens were partially immersed in a 3.5% NaCl solution, and a constant
voltage of 5 V was applied using an external source between the
anode (embedded steel) and the cathode (stainless steel sheet). The
time required for the chlorides to penetrate the material was

Fig. 6. Chloride permeability based on ASTM 1202. (a) Passing charge of concretes with and without coating. (b) Electrical resistivity of concretes with and without coating.

Please cite this article as: Aguirre-Guerrero, A.M., et al., A novel geopolymer application: Coatings to protect reinforced concrete against corrosion,
Appl. Clay Sci. (2016), http://dx.doi.org/10.1016/j.clay.2016.10.029
 A.M. Aguirre-Guerrero et al. / Applied Clay Science xxx (2016) xxx–xxx
Fig. 7. Current intensity versus time for specimens without coatings and with MK/10OPC
and FA/10OPC coatings.
determined based on the current-time intensity curve throughout the
immersion process.
2.4.2.3. Electrochemical measurements. Non-destructive techniques, such
as open circuit potential (OCP) and linear polarization resistance (LPR),
were used to monitor the corrosive behaviour in concretes with and
without coatings. OCP is one of the most widely used procedures during
routine inspections of reinforced structures and is performed in accor-
dance with the ASTM Standard C876 (Standard Test Method for Corrosion
Potentials of Uncoated Reinforcing Steel in Concrete). In this study, OCP
measurements were made using a UNIT-T MODEL UT70A brand
multimeter with a Ag/AgCl electrode. For the LPR measurements, an
electrochemical cell was used with 3 electrodes: a working electrode,
WE (steel embedded in concrete), a reference electrode placed near
Fig. 8. Coated concretes after the impressed voltage accelerated corrosion. (a) Concrete with MK/10OPC coating. (b) Concrete with FA/10OPC coating.
Please cite this article as: Aguirre-Guerrero, A.M., et al., A novel geopolymer application: Coatings to protect reinforced concrete against corrosion,
Appl. Clay Sci. (2016), http://dx.doi.org/10.1016/j.clay.2016.10.029
5
the WE, and a counter-electrode made of stainless steel located near
the concrete. The apparatus used was an Autolab Instrument
PGSTAT128N Potenciostat/Galvanostat. The LPR test was conducted in ac-
cordance with the ASTM Standard G59 (Standard Test Method for
Conducting Potentiodynamic Polarization Resistance Measurements)
while overpotentials of −30 to +30 mV were applied. These measure-
ments were recorded relative to time.
2.4.3. Microstructure
At the end of the exposure of the specimens to impressed voltage,
samples were taken of each of the coatings and microscopically ob-
served using a JEOL brand scanning electron microscope (SEM), Ref:
JSM-6490LV, high vacuum (3 × 10–6 Torr) equipped with an
INCAPentaFETx3 OXFORD INSTRUMENTS brand Detector, MODEL
7573. The samples were coated with gold by deposition in a Denton
VacuumDesk IV vacuum unit.
3. Results and discussion
3.1. Compressive strength of geopolymer mortars
Fig. 4 shows the compressive strength of the geopolymer mortars at
different curing ages. The early strength development of the MK/10OPC
mortar was notable; we attributed this result to the high reactivity of
MK, which allowed for obtaining compressive strength values of up to
40 MPa after 3 days of curing. At the same age of curing, the FA/10OPC
mortar reached compressive strength values of up to 10 MPa. However,
in contrast with the MK/10OPC mortar, its strength development was
continuous over time; at 28 days after curing, the FA/10OPC mortar
reached compressive strength values of up to 43 MPa. The adequate me-
chanical performance of the geopolymer mortars obtained may be due
to the coexistence of two types of gels: the N-A-S-H gel produced by al-
kaline activation of the aluminosilicate precursors (FA, MK) and the C-S-
H gel that results from the hydration of OPC (García-Lodeiro et al., 2012;
6 A.M. Aguirre-Guerrero et al. / Applied Clay Science xxx (2016) xxx–xxx

Mejía et al., 2014; Palomo et al., 2007). Mejía et al. (2015) studied hybrid
cements using fly ash as a precursor at similar molar ratios to those used
in this study. However, they used NaOH + commercial sodium silicate
as the activating solution and an addition of 30% OPC, leading to com-
pressive strength values of 51.7 MPa at the paste level at 28 days. Simi-
larly, Vásquez-Molina et al. (2016) reported strength values of
approximately 30 and 55.6 MPa at 7 and 28 days, respectively, using a
ratio of 80/20 FA/OPC and NaOH + commercial sodium silicate as the
activating solution. This study found lower values for compressive
strength relative to those found by the researchers mentioned previous-
ly, which we attribute to the lower amount of OPC incorporated in the
mixes (10%) and the higher l/s ratio used (0.3). It is worth noting that
even when coatings do not undergo significant demands from a me-
chanical standpoint, the adequate strength development of a coating
is an indirect indicator of its adhesion properties and could be a techni-
cal advantage in structural repair processes and in aiding rapid place-
ment during service conditions.
3.2. Adhesion strength
The substrate-coating adhesion strength was determined using an
Elcometer 106 apparatus, which measured the pull-out of the dolly
fixed on the surface of both coatings. This test was done for the MK/
10OPC and FA/10OPC coatings 7 days after their application. Both
types of coating were found to have very similar adhesion strengths in
the range of 1.5–2.5 MPa; these values are a good match for those ob-
tained by Hu et al. (2008), who reported values of 2.43 MPa after
7 days of curing for a repair mortar based on alkaline-activated MK. Sim-
ilarly, Zhang et al. (2010a) reported values between 1.5 and 2.5 MPa
after 28 days of curing for MK-based coatings. Zhang et al. (2016) re-
ported values between 2 and 2.5 MPa for a mortar based on MK and
FA, though different adhesion measurement methods were used.
Pacheco-Torgal et al. (2008b) used the slant shear test to determine
the strength of adhesion of a geopolymer repair mortar based on mud
from a tungsten mine to the OPC substrate and reported a shear adhe-
sion strength of approximately 16 MPa 5 days after application. Using
the same method, Vasconcelos et al. (2011) reported adhesion
strengths of approximately 0.25 MPa. Similarly, Phoo-ngernkham et al.
(2015) reported values between 11.8 and 26.2 MPa using different
amounts of Portland cement (OPC) added to the geopolymer repair
mortar. These authors concluded that the substrate (concrete) adhesion
strength increases with the content of Portland cement and the concen-
tration of NaOH.
Hybrid geopolymer coatings form C-A-S-H gels, which are similar to
the C-S-H gel formed by cementitious paste but with the inclusion of A1
in the structure; this makes the interface region between the substrate
(OPC concrete) and the GP mortar more homogeneous, achieving a
strong interface between the two materials (Fig. 5). In addition, the

Fig. 9. SEM micrograph after the impressed voltage test (a) FA/OPC coating (left) and (b) MK/10OPC coating (right).

Please cite this article as: Aguirre-Guerrero, A.M., et al., A novel geopolymer application: Coatings to protect reinforced concrete against corrosion,
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 A.M. Aguirre-Guerrero et al. / Applied Clay Science xxx (2016) xxx–xxx
calcium hydroxide present in the OPC substrate may react with the A1
and Si elements in the geopolymer paste due to the Ca2+ balance effect
(Pacheco-Torgal et al., 2008b); the increased amounts of these reaction
products improve the interface region between the GP coating and the
concrete substrate. Therefore, the geopolymer coating can exhibit
strong adhesion to the OPC substrates. Fig. 5 shows that the FA/10OPC
coating exhibits greater porosity compared to the MK/10OPC coating,
which looks denser and appears to have smaller pores.
3.3. Permeability to chloride ions
The permeability to chloride ions was measured in accordance with
the passing charge during the permeability test (ASTMC 1202); these
values can be seen in Fig. 6a. The concrete specimens without coating
exhibited higher charge values compared to the coated concrete speci-
mens. The FA/10OPC coating exhibited the lowest charge value of the
two types of coatings evaluated (under 1000 C), which indicated “very
low” chloride permeability. The concrete specimens coated with MK/
10OPC also exhibited good performance against chlorides, placing
them in the “low” permeability range. Fig. 6b shows the electrical resis-
tivity, which was calculated using the chloride permeability test. The
coated concrete specimens exhibited higher electrical resistivity com-
pared to the concretes without coatings. Different authors (Bernal et
al., 2012; Ismail et al., 2013; Zhu et al., 2014) have observed a reduction
in chloride permeability in geopolymers compared to OPC concrete due
to reductions in porosity and pore size and an increase in tortuosity,
which are due mainly to the dense structure of the gel (C,N)-A-S-H
and its coexistence (Ismail et al., 2013). However, these studies have
all been conducted on bulk materials and not for coated concretes, as
in the present study.
3.4. Corrosion tests
3.4.1. Impressed voltage
Fig. 7 shows the current intensity versus time curve for the speci-
mens with and without coatings. The concretes with coating exhibited
an initial current that was much lower compared to the initial currents
Fig. 10. Corrosion test (wetting/drying cycles) for specimens without coating and with FA/10OPC and MK/10OPC coatings. (a) Behaviour of open circuit potential, (b) behaviour of Icorr and
(c) visual inspection of steel embedded in concrete after the final exposure to chlorides (cycle 10).
Please cite this article as: Aguirre-Guerrero, A.M., et al., A novel geopolymer application: Coatings to protect reinforced concrete against corrosion,
Appl. Clay Sci. (2016), http://dx.doi.org/10.1016/j.clay.2016.10.029
7
of the concretes without coating. This current remained constant until
after approximately 3.5 h of accelerated chloride exposure, and then, a
significant increase in the current occurred. After 130 h of exposure,
the concrete with the FA/10OPC coating exhibited the highest current
compared to the other specimens. The onset of the first cracks between
all specimens occurred at similar times: for FA/10OPC, the first crack oc-
curred at 161.7 h; for MK/10OPC, the first crack was observed at 157.4 h;
and without coating, the first crack occurred at 156.2 h. The observa-
tions made during the accelerated impressed voltage test suggested
that coatings protect the material against chloride corrosion during
the time required for chloride ions to penetrate the coating, which
was seen in the initial phase of the test, in which the first 3 h of the ac-
celerated test exhibit very low currents for concretes with coating. Once
the coating barrier was overcome, the chloride ions continued their dif-
fusion through the cementitious matrix, which explains why similar
values were encountered for the onset of the first cracks in all specimens
(Fig. 8). It is important to note that this method involves an accelerated
chloride inclusion process for the system, which significantly exceeds
any condition of real exposure because the experimental setup depends
on the reinforcing steel behaving in an anodic manner.
The concrete with the MK/10OPC coating exhibited a lower current
value, suggesting that the material has a higher electrical resistance
(Reddy et al., 2011) compared to the rest of the specimens. One could
conclude that the concrete with the MK-based geopolymer coating ex-
hibits better behaviour against corrosion of the reinforcing steel.
Currently, the literature does not include any results on geopolymer
coatings applied to concrete specimens subjected to accelerated
impressed voltage tests. However, Kriven et al. (2009) found that con-
crete reinforced with steel bars that were previously coated with an
MK-based geopolymer showed an increase in corrosion resistance due
to the coating; without coating, the steel took 7 days to reach a 25% cor-
rosion level, while the coated steel took 17 days to reach the same level
of deterioration. In addition, Olivia and Nikraz (2010) reported that con-
crete based on alkaline-activated FA showed an increase in corrosion re-
sistance compared to OPC concretes; in that experiment, it took longer
for the onset of the first crack in the geopolymer concrete. In addition,
they reported that these concretes exhibit lower electrical resistance
8 A.M. Aguirre-Guerrero et al. / Applied Clay Science xxx (2016) xxx–xxx
compared with OPC concretes. The structure of the (C,N)-A-S-H gels
present in these hybrid geopolymer materials is said to have a tortuous
nature (García-Lodeiro et al., 2012), which leads to a more complex
diffusion pattern of chloride ions. Thus, during the initial phases of the
test, very low currents were encountered due to the action of the
geopolymer coatings; this finding is in agreement with previously pre-
sented permeability tests.
Fig. 8 shows the concrete specimens after the impressed voltage test.
It can be seen that lixiviation of corrosion products occurred; however,
large cracks were not observed in the concrete, so it can be suggested
that there were microcracks inside the concrete. Fig. 8b shows that
the FA/10OPC coating was cracked and exhibited visible delamination
from the substrate. After the impressed voltage test was conducted,
coated samples were obtained for microstructural observation. Fig. 9
shows the SEM images of the FA/10OPC and MK/10OPC coatings. It
can be seen that in both coatings, there were cracks and porosity. The
cracks may act as conductive channels and may promote the diffusion
of chloride ions, which suggests the possible deterioration of the coating
during the accelerated exposure to chlorides; this finding explains why
the protective effects of these coatings decay over time. It is worth
highlighting that a good interface can be observed between the PP
fibre and the GP matrix in both coatings. It can also be seen that the
MK/10OPC coating is more compact and dense than the FA/10OPC
coating.
3.4.2. Wetting/drying cycles
Fig. 10a shows the behaviour of the open circuit potential for the
specimens with and without coating. At the initial time point (0 cycles),
the concretes with and without coating exhibited a 10% probability of
corrosion, which corresponds to the passive state of the reinforcing
steel bars.
Starting at cycle 2, it was observed that the potentials became much
more negative for all specimens as a result of chloride exposure; howev-
er, for the specimen with the MK/10OPC coating, the potential was
much more positive compared to the FA/10OPC-coated and uncoated
concretes. This behaviour can be readily observed from cycles 2 to 4,
moving into the region of uncertain probability of corrosion. Starting
at cycle 5 until the end of the exposure, all specimens exhibited very
similar behaviours, with much more negative potentials and corrosion
probabilities of 90%. This technique suggests the corrosive state of the
reinforcing bars, though it is not a quantification of corrosion. Therefore,
corrosion velocities were calculated using the linear polarization tech-
nique (LPR).
LPR has been widely applied since the 1970s to obtain quantitative
information on corrosion velocity (Bertolini et al., 2004; Montemor et
al., 2003; Song and Saraswathy, 2007). The calculation of the corrosion
current was done by applying the Stern-Geary formula:
B 3. The resistance of chloride permeability of both geopolymers-based
Icorr ¼
Rp
where B is a constant that depends on the Tafel slopes, whose estimated
value is 26 mV or 52 mV depending on the active or passive state of the
steel. In this study, the value “B″ used was 0.026 V, which simulates the
active corrosion condition (Andrade and Alonso, 1996; Andrade and
González, 1978).
Fig. 10b shows the current densities for the specimens with and
without coatings exposed to w/d cycles. It can be seen that the Icorr
values for the MK/10OPC-coated specimens from cycles 1 to 4 were
much lower compared to the values for the specimen without coating,
in which the steel remained in its passive state. For the FA/10OPC-coat-
ed specimen, the Icorr values were lower compared to the uncoated
specimen from cycles 1 to 2, though after cycle 3, the Icorr values
were very similar to those of the uncoated specimen. From cycle 5 to
the end of the exposure, the corrosion velocities of all specimens were
very similar. The application of the geopolymer coating significantly
Please cite this article as: Aguirre-Guerrero, A.M., et al., A novel geopolymer application: Coatings to protect reinforced concrete against corrosion,
Appl. Clay Sci. (2016), http://dx.doi.org/10.1016/j.clay.2016.10.029
improved the performance against corrosion in the early cycles, which
suggests that chloride ions are able to diffuse through the coating after
the first few cycles (MK/10OPC up until cycle 4, FA/10OPC up until
cycle 2). Afterwards, the chloride ions reach the OPC cementitious ma-
trix, where their diffusion is very similar. At the end of the w/d cycles,
all the specimens were in a high corrosion state. This behaviour is sim-
ilar to that observed for impressed voltage.
The application of geopolymer coatings to concrete can reduce the
penetration of chloride ions and improve the durability of concrete
(Wiyono et al., 2015); until chlorides can penetrate the coating, as
seen in the results of this study. The MK/10OPC coating had the best per-
formance; Fig. 5 shows that this was a denser and more compact mate-
rial relative to FA/10OPC. Zhang et al. (2010b) suggested the use of
coatings based on the alkaline activation of MK as an anticorrosive ma-
terial, a characteristic that is promoted by its low porosity and, there-
fore, its resistance to the penetration of aggressive ions. Though this
study corroborated the good performance of the MK coating, this poly-
mer has a useful lifetime; in the case of MK/10OPC, this parameter
reaches a maximum after the first 4 w/d cycles. Kupwade-Patil and
Allouche (2012) exposed geopolymer concretes based on alkaline-acti-
vated FA to seawater for a year and observed a small increase in poros-
ity. One could suggest that the GP material, after undergoing the w/d
cycles, may slightly increase in porosity and therefore facilitate the pen-
etration of chloride ions. If this were the case, it could explain the behav-
iour after the 5th w/d cycle.
Fig. 10c shows the visual inspection of the steel embedded in the
specimens after the last exposure period. In general, the steel was clear-
ly affected by localized corrosion in all cases. The appearance of the steel
is typical of pitted corrosion attacks, as is commonly seen with
chlorides.
4. Conclusions
The use of two hybrid geopolymer coatings was proposed as a possi-
ble protective element for reinforced concrete structures exposed to
marine environments. Based on the results presented herein the follow-
ing conclusions can be derived:
1. The results indicated that the early compressive strength of MK/
10OPC mortar was higher than the CV/10OPC mortar, because of
the high reactivity of MK.
2. Both coatings MK/10OPC and CV/10OPC exhibit good adhesion
strengths on concrete substrate, due to the hybrid geopolymer coat-
ings form C-A-S-H gels, which are similar to the C-S-H gel formed by
cementitious paste but with the inclusion of A1 in the structure; this
makes the interface region between the substrate (OPC concrete)
and the GP mortar more homogeneous.
ð1Þ
coatings system was superior to the concrete without coating. The
coated concrete specimens exhibited higher electrical resistivity
compared to the concretes without coatings.
4. The evaluation of the corrosive process through the use of accelerat-
ed techniques suggests that geopolymers can be used as protective
coatings for concretes exposed to chlorides. Of the coatings evaluat-
ed, the coating based on metakaolin (MK + OPC) exhibited the
best performance. However, both coatings evaluated had the same
protection durability (useful lifetime); in this case, the use of acceler-
ated methods, whose conditions exceed those found under real life
exposure conditions, showed that the maximum time was 4 w/d cy-
cles for the metakaolin (MK)-based geopolymer coating.
5. We recommend further research with less severe conditions
given the excellent characteristics exhibited by the coatings,
which include their mechanical strength, chloride permeability,
electrical resistivity and adhesion capacity to the concrete surface
(substrate).
 A.M. Aguirre-Guerrero et al. / Applied Clay Science xxx (2016) xxx–xxx
Acknowledgements
The authors and members of the Composite Materials group express
their appreciation in particular to Engineer Johanna Mejía for her valu-
able contributions to the experiment, to the Institute of Development,
Science, Technology and Innovation (Colciencias) for the support re-
ceived under the framework of the “HYBRICEMENT” project within
the contract 0638-2013, to Universidad Del Valle (Cali, Colombia) and
to the Centre of Excellence in New Materials (CENM) for the support
provided in developing this study. The authors thank GENSA for provid-
ing the fly ash and BASF for providing the metakaolin used in this re-
search project.
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