Construction and Building Materials 275 (2021) 122120

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Construction and Building Materials

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

Determination of shear strength by Iosipescu (V-notch) method

of metakaolin-based geopolymeric resins activated by different silicate
and hydroxide combinations
Joadelio Chagas Soares a,⇑, Dylmar Penteado Dias a, Eduardo Atem de Carvalho b,
Jodimar Soares de Azevedo a
a
Civil Engineering Laboratory of Universidade Estadual do Norte Fluminense Darcy Ribeiro, Av. Alberto Lamego, 2000 Parque Califórnia, Campos dos Goytacazes, RJ CEP:
28013-602, Brazil
b
Advanced Materials Laboratory of Universidade Estadual do Norte Fluminense Darcy Ribeiro, Av. Alberto Lamego, 2000 Parque Califórnia, Campos dos Goytacazes, RJ CEP:
28013-602, Brazil

h i g h l i g h t s

Evaluation of physical and mechanical properties of metakaolin-based geopolymeric resins.

Variations in alkaline-activating solution influenced the consistency and setting times.

Shear strength and shear modulus of all geopolymeric resins tested reached favorable results by Iosipescu test.

Slightly denser and more homogenous matrix were found in geopolymeric resins activated by potassium hydroxide.

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

Article history: Geopolymers (inorganic polymers) were developed and patented by Joseph Davidovits in the 1970’s and
Received 6 July 2020 have gained significant attention in the civil construction industry. Since then, the properties of geopoly-
Received in revised form 11 December 2020 mers have been studied by many researchers, such as their use as a repair material on reinforced concrete
Accepted 20 December 2020
structures. Thus, this study aimed to evaluate the mechanical properties of metakaolin-based repair
Available online 9 January 2021
geopolymeric resins. The geopolymeric resins were prepared with alkaline activators composed by
sodium and potassium silicates combined to sodium and potassium hydroxides to determine the prop-
Keywords:
erties of fresh mixtures (workability, setting times), the adhesion coefficient at the interface substrate/
Geopolymeric resin
Compressive strength
resin and the gain in compressive and indirect tensile strengths up to 28 days of age. The Iosipescu or
Iosipescu test V-Notch shear tests were used to determine the shear strength and shear modulus, according to ASTM
Shear strength D 5379 (1998) specifications, as these are the most important mechanical properties when studying
structural repairs. The results indicated that all geopolymeric resins achieved high mechanical strength
in the early ages, which is fundamental for structural repair applications. The gain in compressive
strength ranged from 60% on the first day to 85 to 93% after 3 days when compared to the results
obtained at 28 days of age. All resins reached compressive strengths greater than 80 MPa and indirect
tensile strengths between 5 and 6 MPa at 28 days of age. The shear strength (s) values were around varied
from 4.31 to 7.55 MPa. The resins with combination of sodium silicate with potassium hydroxide and
potassium silicate with sodium hydroxide showed higher shear moduli, being respectively 6,13 and
8,20 GPa. The results obtained show that the resins developed in this work have enormous potential
for use in repairing reinforced concrete structures.
Ó 2020 Elsevier Ltd. All rights reserved.

1. Introduction

In the past few decades, many researchers have tried to develop

alternative materials to Portland cement. Geopolymer cement is
⇑ Corresponding author. one of them, being a material made up of aluminosilicates with
E-mail address: joadelio.soares@iff.edu.br (J.C. Soares). amorphous structure to semicrystalline activated by a highly

https://doi.org/10.1016/j.conbuildmat.2020.122120
0950-0618/Ó 2020 Elsevier Ltd. All rights reserved.
Joadelio Chagas Soares, Dylmar Penteado Dias, Eduardo Atem de Carvalho et al.
alkaline solution of silicates and/or hydroxides [1]. The reaction
mechanism is called geopolymerization and, according to Van
Jaarsveld et al. [2], it requires a strong alkaline medium to dissolve
silica and/or alumina and hydrolyze the particle surface of the raw
material (precursor).
There are several types of alkaline activators that can be used in
the geopolymerization process, e.g. alkaline sodium silicate (Na2-
SiO3), potassium silicate (K2SiO3), sodium hydroxide (NaOH),
potassium hydroxide (KOH) and calcium hydroxide [Ca(OH)2] [3–
8]. Leong et al. [7] reported that the combined use of Na2SiO3
and NaOH is the most common practice in terms of cost-
efficiency to produce geopolymers with higher compressive
strength than the exclusive use of silicates or hydroxides.
Geopolymers have excellent properties, such as high initial and
final mechanical strengths, low shrinkage, good steel-geopolymer
adherence, aggressive agents and high temperature resistance
[9,10]. Structural strengthening in concrete beams consists in
applying epoxy resin-based adhesives to improve bonding
between the components. To be considered suitable for use as rein-
forcement, the adhesive material must have sufficient stiffness
modulus, good workability, low shrinkage during the curing pro-
cess and excellent adhesive properties with concrete and steel
bars. Recent studies have verified the adhesive properties of
geopolymers for structural repair applications [11,12]. However,
there are still many questions about geopolymeric materials to
be answered, despite the increased number of promising
researches by the international community related to manufactur-
ing, mechanical properties and durability [13,14].
Geopolymer cement is an innovative material and recent studies
[15–18] have drawn attention to its great performance in construc-
tion applications. These structure designs require a high understand-
ing of the material’s mechanical properties for reliable application.
Therefore, one of the most important properties in structural calcula-
tions is the shear modulus and shear strength [19–21]. Nevertheless,
the shear behavior of geopolymeric materials has not been fully
understood, because there is not an adequate and accurate direct
shear test method. Several methods have been developed to measure
shear properties of materials, such as 45° shear, asymmetric four-
point bending(AFPB) and short beam shear (SBS) [22]. Oneof the most
popular tests is the Iosipescu method (V-notch), which has clear and
recognized procedures by the American Society for Testing and Mate-
rials (ASTM) since 1993. The principle of the Iosipescu method is
based on a simple four point bending test.
Most of shear tests show inconsistent results, since the specimens’
cross-sectional area are not in pure or non-uniform shear states. For
this reason, the Iosipescu shear test [23] was widely used to deter-
mine the shear properties, mainly of composite materials [24,25].
Even so, academic works and applications in the industry are limited
and most research is focused on laminated composites [22].
Therefore, the main purpose of this study is to produce four
types of metakaolin-based geopolymer resins activated by differ-
ent alkaline activators combined with each other (Na2SiO3 + NaOH,
Na2SiO3 + KOH, K2SiO3 + NaOH and K2SiO3 + KOH). The compres-
sive strength and indirect tensile strength of the resins were deter-
mined. The Iosipescu method (V-notch) was adopted to obtain the
shear strength parameters, shear modulus, strain and failure
modes of the four geopolymeric resins and a commercial epoxy
resin for comparative reasons.
2. Materials and methods
2.1. Raw materials
The geopolymeric resins were produced by mixing a precursor
material, an alkaline-activating solution and a fine aggregate. The
2
Construction and Building Materials 275 (2021) 122120
precursor was metakaolin, which is a pozzolanic material basically
consisting of silica (SiO2) and alumina (Al2O3). Its specific mass and
chemical composition, obtained by X-ray fluorescence, are shown
in Table 1. The granulometry assay was used to determine the pre-
cursor particle size distribution (Table 2). The alkaline activating
solutions were manufactured by combining sodium hydroxide
(NaOH), potassium hydroxide (KOH), alkaline sodium silicate (Na2-
SiO3) and potassium silicate (K2SiO3), as shown in Table 3. The
chemical compositions in Table 4 were provided by the manufac-
turers. The alkaline-activating solutions correspond to the specific
molar ratios, as shown in Table 5. The fine aggregate used was a
fine quartzite sand standardized by the Institute for Technological
Research of the State of São Paulo (IPT), sieve n° 100 (opening size
0.075 mm) and fineness modulus of 1.75, as established in NBR
7214 [26]. There are several types and brands of epoxy resins in
the Brazilian market. It was selected a resin with characteristics
and mechanical properties close to the geopolymeric resins made
in this work. The chosen commercial epoxy resin had a compres-
sive strength of 60 to 70 MPa at 28 days.
2.2. Resin manufacturing
The geopolymeric resins were obtained by mixing the precursor
(metakaolin) with the alkaline-activating solution. First, metakao-
lin and fine sand were weighed and mixed. The alkaline-activating
solutions were mixed for 5 min and were produced 24 h before the
specimens being molded. The resins were manufactured in a plan-
etary mixer SOLOTEST model GC 15, with maximum capacity of 5L.
The alkaline-activating solution, metakaolin and fine sand were
added to the mixer machine and blended together for 6 min:
2 min at low speed (140 ± 5 rpm), followed by 4 min at high speed
(285 ± 10 rpm). Finally, the resins were poured into Ø
50 mm  100 mm cylindrical casts for mechanical tests and into
acrylic molds for Iosipescu shear tests. Consistency and setting
time tests were carried out by flow-table method and Vicat needle
test, respectively. The tests were conducted according to standards
NBR 13276 [27] and NBR 16607 [28]. After 24 h, the specimens
were demolded and cured at room temperature (23 ± 0.5 °C) and
at humidity of 80%. Thermal curing and water submersion were
not performed since the increase in mechanical resistance at early
ages was high enough to be compatible to materials used in struc-
tural repairing. The commercial epoxy resin was produced accord-
ing to manufacturing specifications.
2.3. Tensile strength of the interface
Splitting tests were performed according to NBR 7222 [29] to
evaluate the adhesion between Portland cement and the geopoly-
meric resins produced. The results were also compared to commer-
cial epoxy resins. Mixed cylindrical specimens with dimensions of
Table 1
Physical and chemical characteristics of metakaolin.
Chemical composition Weight
Al2O3 (%) 47.20
SiO2 (%) 44.49
Fe2O3 (%) 3.76
K2O (%) 1.68
SO3 (%) 1.30
TiO2 (%) 1.28
CaO (%) 0.06
Specific mass (g/cm3) 2.57
Loss on ignition (%) 2.50
Joadelio Chagas Soares, Dylmar Penteado Dias, Eduardo Atem de Carvalho et al. Construction and Building Materials 275 (2021) 122120

Table 2 mechanical testing machine with 1000 kN capacity at a loading

Particle size of metakaolin. rate of 0.3 MPa/s. For each resin, three Ø 50 mm  100 mm spec-
Diameter Sample (lm) imens were also tested to determine the indirect tensile strength,
D10 0.6 according to NBR 7222 [31], at the age of 28 days. The recommen-
D50 12.9 dations of ASTM C 1231 [32] were followed, ensuring the applied
D90 47.3 loads were uniformly distributed.
Dmédio 20.3

2.5. Modulus of elasticity

Table 3
Three cylindrical specimens of Ø 50 mm  100 mm were tested
Geopolymeric resin nomenclature and activating compounds.
in a universal testing machine with 100 kN capacity and loading
Geopolymeric resin Silicate Hydroxide rate of 0.5 mm/min to determine the modulus of elasticity. The
S.s – S.h Na2SiO3 NaOH loading and strain values were obtained using a Vishay P3 data
S.s – P.h Na2SiO3 KOH acquisition system. The modulus of elasticity and the Poisson’s
P.s – S.h K2SiO3 NaOH
ratio were calculated according to NBR 8522 [33].
P.s – P.h K2SiO3 KOH

2.6. Shear strength

Ø 50 mm  100 mm were molded in two steps. The first step con-
sisted in filling the molds with Portland cement concrete with aid
of metallic shields on their symmetry axis. The specimens were
demolded 24 h later and placed into curing tanks for 28 days. After
curing process, they were exposed to room temperature (23 °C ± 0.
5 °C) and at humidity of 80% during 24 h for drying, sanding and
cleaning. The second step consisted in placing back half of the sub-
strate specimens into the cylindrical molds, and filling the other
half with different types of resin. Fig. 1 shows the equipment used
in the production of mixed specimens for splitting tests.
The adhesion coefficient (a) can be defined as the ratio between
the mean tensile strength at interface (f tim ) and the mean tensile
strength of weakest material (substrate or resin) (f ctm ) Eq.(1).
f tim
a¼
f ctm
Three specimens with dimensions of Ø 100 mm  200 mm were
produced for compressive tests (NBR 5739) [30] and three other
specimens were made for tensile tests (NBR 7222) [31]. For the
splitting test, three specimens were molded for each resin type.
The samples were tested in a universal machine Shimadzu model
UH of 500 kN capacity at a loading rate of 2 kN/s, as shown in Fig. 1.
2.4. Mechanical tests
Three cylindrical specimens of Ø 50 mm  100 mm of each geo-
polimeric resin were tested for compression strength, according to
NBR 5739 [30], at the ages of 1, 3, 14, 28 and 90 days, in a universal
Table 4
Chemical composition of silicates and hydroxides.
Component (%) H2O SiO2 Na2O
Na2SiO3 53.00 32.65 15.17
K2SiO3 59.75 27.29 – 12.86
NaOH 21.90 – 75.20
KOH 12.90 – 87.10
The shear behavior of geopolymeric resins and commercial
epoxy resin was evaluated by the Iosipescu test (V-notched speci-
men), according to the specifications of ASTM D 5379 [23]. Five
specimens being 76 mm long, 20 mm wide and 8 mm thick were
molded for each resin type (Fig. 2). The upper and lower edges of
specimens were machined to become flat planes, parallel to each
other and perpendicular to the specimen faces, in order to avoid
out-of-plane bending and twisting when the load is applied.
Two opposite 1.3 mm radii notches were cut into the specimen
symmetry axis to induce and control the uniformity of the shear
stress field. The samples were inserted into the device with the
notches located along the loading line by an alignment device pre-
sent at loading device. The two halves of the device were com-
pressed by an universal testing machine with 100 kN capacity
ð1Þ
(Fig. 3) and a loading rate of 2 mm/min, leading to a relative dis-
placement while the loading was monitored. To measure the strain
of the specimens, a 45° strain-gage was bonded to the net ligament
between the two notches (Fig. 3). According to ASTM D 5379 [23],
the loading involved in the test can be idealized as asymmetric
bending, as shown in the shear diagrams and bending moment in
Fig. 4.
A Finite Element model was constructed to simulate the Iosi-
pescu specimen used in this work and a commercial software
was used afterwards. Given the non-symmetric nature of the load-
ing/clamping, a full specimen model was used. 16 surfaces were
imposed, 8 each side of the notch axis. Mesh for this model was
refined progressively inside the surfaces, and those close to the
notches were refined the most. Convergence were achieved using
24,176 plane-strain, solid, 2D elements containing 96,551 nodes.
ASTM D 5379 [23] points to a ±45° uniaxial type strain gage
bonding, but this solution is geared to composite materials, where
K2O
directions matters. In this case, the studied material is homoge-
– neous and isotropic and this makes the use of a second strain
redundant, so this work opts for the use of a single strain gage.
–
ASTM D 5379 [23] recommends the use of a minimum sized
strain gage, given the nature of the intended studied material,

Table 5
Molar ratios of alkaline activator solutions.

Geopolymeric resin Molar ratio

SiO2/Al2O3 H2O/*M2O *M2O/SiO2 *M2O/Al2O3
S.s – S.h 1.97 2.37 0.31 0.62
S.s – P.h 1.97 2.16 0.34 0.66
P.s – S.h 1.89 2.56 0.31 0.59
P.s – P.h 1.89 2.33 0.33 0.63
*
M = Na or K.

3
Joadelio Chagas Soares, Dylmar Penteado Dias, Eduardo Atem de Carvalho et al. Construction and Building Materials 275 (2021) 122120

Fig. 1. a) Metal molds; b) Mixed specimens; c) Test set-up for splitting tests in substrate/geopolymeric resin interface; d) Test set-up for splitting tests substrate/commercial
epoxy resin.

composites. The goal is to minimize the gradient captured by strain The shear strain c12 was obtained by reading the strain gage at
gage grid. The Finite Element simulation for the homogeneous, iso- 45° (a single-element gage mounted) and is calculated using Eq.
tropic, elastic material has shown that exists a constant shear value (3).
area of a roughly diamond-shaped area, touching the notches
roots, with the width about 12 mm. This could easily house the
c12 ¼ 2jeð45 Þj ð3Þ
strain gage used in this work. The shear modulus is calculated by Eq. (4).
The shear strength in the V-notched cross-sectional area is cal-
culated using Eq. (2). G12 ¼ Ds=Dc ð4Þ

where Ds is the difference in applied shear stress between the two

s ¼ P=A ð2Þ strain points and Dc is the difference between the two strain points.

where P is the load applied and A is the cross-sectional area 2.7. Scanning electron microscopy (SEM)
between the notches.
The microstructural analysis of geopolymeric resins and com-
mercial epoxy was carried out on the fracture surfaces from the
Iosipescu test specimens. The equipment used to obtain the images
was a Shimadzu scanning electron microscope, model SSX-550,
operating at 20 keV.

3. Results and discussions

3.1. Workability

Workability of mortar is the main property in the fresh state,

and it can be estimated by consistency. A material with adequate
Fig. 2. Geometry and dimensions of Iosipescu specimen. workability provides ease of handling, application and surface reg-
4
Joadelio Chagas Soares, Dylmar Penteado Dias, Eduardo Atem de Carvalho et al.
Fig. 3. (a) Instrumented specimens using strain gage at 45°; (b) Test set-up for determination of shear strength (Iosipescu method).
Fig. 4. Loading of an Iosipescu specimen with shear force and bending moment
diagrams (adapted from ASTM D 5379, 1998).
ularization. When the workability is not adequate, the mortar can
be very dry, rough or excessively fluid. These factors compromise
its application. It may also show segregation, excessive exudation
or low adherence to substrate.
The consistency index of geopolymeric resins is shown in Fig. 5.
Geopolymeric resins showed good workability. However, resins
produced with potassium hydroxide were more fluid than those
produced with sodium hydroxide. It was observed the consistency
5
Construction and Building Materials 275 (2021) 122120
Fig. 5. Consistency index of geopolymeric resins.
index was higher for the same type of silicate when using KOH in
the composition. According to Leong et al. [34], this is due to the
greater solubility of potassium in relation to sodium. The silicates
used in the mixtures reduced workability by virtue of their viscous
nature, especially Na2SiO3 (alkaline sodium silicate) which has
lower amount of H2O in its composition than K2SiO3 (potassium
silicate). By contrast, hydroxides (NaOH and KOH) are fluid in nat-
ure and increase workability according to Rangel [35].
3.2. Setting times
Setting time is affected by many factors such as the nature of
pozzolanic material, temperature, mixing ratio, alkaline activators
and water content [36]. Fig. 6 shows the initial and final setting
times of the geopolymeric resins produced. Initial setting times
ranged from 40 to 87 min and the final ones ranged from 66 to
113 min. The resins activated with potassium hydroxide showed
longer initial and final setting times. Saloma et al. [37] found val-
ues of 88 and 135 min for initial and final setting times, respec-
tively, in geopolymeric mortars activated with NaOH and
molarity equal to 16 M. Khan et al. [38] produced fly-ash based
Joadelio Chagas Soares, Dylmar Penteado Dias, Eduardo Atem de Carvalho et al. Construction and Building Materials 275 (2021) 122120

geopolymer activated by NaOH and obtained values of initial and Table 6

final setting times of 90–250 min. Adhesion coefficient at the substrate/resin interface.

The mixing ratios are presented in Table 5. It was noticed that Specimen Adhesion coefficient (a)
Si/Al ratio and H2O/Solids ratio are almost the same for different Substrate/S.s – S.h resin interface 0.57 ± 0.09
solutions. However, S.s - S.h resin composition exhibited a shorter Substrate/S.s – P.h resin interface 0.60 ± 0,02
setting time than P.s - P.h resin. According to Chang [39] and Kara- Substrate/P.s – S.h resin interface 0.63 ± 0.05
coka et al. [40], Na+ content is the main factor that influences set- Substrate/P.s – P.h resin interface 0.56 ± 0.06
Substrate/commercial epoxy resin interface 0.66 ± 0.06
ting time because Na+ works as reaction catalysts.
Initial setting time represents the moment at which the mate-
rial reaches a considerable increase in its consistency and, conse-
quently, loses workability and no longer must be handled. The weight aggregate concrete interfaces with values 30% to 200%
geopolymeric resins produced with potassium hydroxide exhibited higher. This demonstrates that mechanical strength is a primary
longer setting times. This is an advantage to other resins produced property for adhesion performance in addition to the surface
with sodium hydroxide because it permits the resin to be longer roughness.
handled prior application onto the substrate. The final setting time Fig. 7 shows the rupture mode of specimens. The rupture occurs
is represented by total solidification with considerable strength due to loss of adhesion and it occurs exactly at the interface of the
gains in the first hours which is an important fact in structural two materials along the loading line.
repair services.
3.4. Mechanical properties

3.3. Adhesion coefficient of the interface

The results of compressive strength as a function of time for the
four geopolymeric resins are shown in Fig. 8. The values obtained
The adhesion coefficient (a) was calculated using Eq. (1) and its
are compatible with the strength curves proposed in the literature
values are shown in Table 6. The average values of the adhesion
[8,42–44]. As expected, resins in the early ages showed high gains
coefficient of the substrate/geopolymer resin interface ranged from
in mechanical strength. The gains were about 60% after 1 day and
0.57 to 0.63. These results were very close to the value of 0.66
ranged from 85 to 93% after 3 days, in comparison to the compres-
found for the substrate/commercial epoxy resin interface. The
sive strength at 28 days. This is due to the high amount of precur-
geopolymeric resin interfaces manufactured with mixed alkaline
sor available for reactions in the early days. At 90 days, the resins
solution (S.s - P.h and P.s - S.h) showed higher values than those
had a lower gain in mechanical strength, except for S.s - P.h resin,
produced with non-mixed solution (S.s - S.h and P.s - P.h). The sub-
which was approximately 17%.
strate/resins surface roughness of all specimens was low, i.e., the
Ambily et al. [45] developed a granulated blast-furnace slag and
surfaces are smooth. Therefore, the adhesion at the interface was
active silica-based ultra-high performance geopolymeric concrete,
almost exclusively due to the adhesion between the resin and
cured at room temperature. The compressive strength found at
the substrate.
early ages were approximately 50% and 78% after 7 days, compared
Costa et al. [41] studied the adhesion of interfaces between nor-
to the strength at 28 days. This high strength in the early ages is
mal density concrete and lightweight aggregate concrete. It was
essential in structural repair works.
observed that greater mechanical strength of the bonding materi-
Nath and Saker [21] investigated the mechanical strength of
als leads to greater tensile strength at the interface. They also con-
low-calcium fly ash-based geopolymeric concrete, cured at room
cluded that smoother surfaces have less friction and, consequently,
temperature. The results showed that the compressive strength
less adherence. Costa et al. [41] produced mixed cylindrical speci-
increased from 15 to 30% after 90 days, compared to the strength
mens with combined interfaces between normal specific weight
at 28 days, indicating gains in mechanical strength for ages after
concrete and lightweight aggregate concrete. Concretes showed
than 28 days.
average compressive strength value of 50–75 MPa and tensile
The indirect tensile strength of metakaolin-based geopolymeric
strength of 3–5 MPa. The smooth interfaces exhibited an adhesion
resins at 28 days is shown in Table 7. The values ranged from 6.8 to
coefficient varying from 0.21 to 0.44. It was observed that sub-
7.1% with respect to the compressive strength at 28 days. These
strate/geopolymeric resins and commercial epoxy resin interfaces
results were compared with theoretical values obtained by mathe-
showed better performance than normal specific weight and light-
matical equations proposed by Nguyen et al. [46], also with the
standard NBR 6118 [47] and the experimental results obtained
by Rocha et al. [8] for metakaolin-based geopolymeric mortars
activated by silicates and hydroxides, whose values ranged
between 4.9 and 6.1%.
Nguyen et al. [46] proposed Eq. (5) for calculating the indirect
tensile strength (f ct ) of fly ash-based mortars.
qffiffiffiffiffiffiffi
f ct ¼ 0:7  f cm ð5Þ

where f cm is the compressive strength, in MPa.

For Portland cement concrete with compressive strength
between 55 and 90 MPa, not having sufficient experimental data,
NBR 6118 [47] establishes that the average indirect tensile
strength (f ctm ) must be calculated using Eq. (6).
f ctm ¼ 2:12  lnð1 þ 0:11  f ck Þ ð6Þ
where f ck is the compressive strength of the concrete, in MPa.
Table 7 shows that the theoretical values calculated were sim-
Fig. 6. Initial and final Setting times of the geopolymeric resins. ilar to the results obtained experimentally in this study. In Fig. 9,
6
Joadelio Chagas Soares, Dylmar Penteado Dias, Eduardo Atem de Carvalho et al. Construction and Building Materials 275 (2021) 122120

Fig. 7. (a) Adhesive failure at the substrate/geopolymeric resin interface; (b) Adhesive failure at the substrate/commercial epoxy resin interface.

intermediate values for elastic modulus. Mazza [51] and França

Fig. 8. Compressive strength of metakaolin-based geopolymeric resins.
it is possible to observe that the specimens tested for compression
and indirect tensile showed failure mode similar to conventional
concrete specimens.
3.5. Modulus of elasticity
The modulus of elasticity of geopolymers depends on several
properties related to chemical composition, microstructure, time
and curing temperature [48–50]. It was obtained by the tests in
the elastic regime, considering 40% of the rupture load. The results
are shown in Table 8. The results show that the modulus of elastic-
ity of S.s - S.h resin was 17% higher compared to S.s - P.h resin
while the elastic modulus of P.s - S.h resin was about 19% higher
than P.s - P.h resin. Geopolymeric resins produced with mixed
alkaline activating solutions (S.s – P.h and P.s – S.h) exhibited
[52] found values between 10.5 and 17.1 GPa in their studies on
metakaolin-based geopolymer mortars. However, these values
were lower when compared to those obtained for Portland cement
concrete. Repair materials with high stiffness should be avoided as
they can create unexpected stress concentrations in the repaired
area [53]. Thus, less stiff geopolymeric resins are advantageous
for structure rehabilitation since they have greater deformation
states without causing cracking the substrates. Therefore, the elas-
tic properties are determining parameters when choosing a repair
material and it side with the good performance of repair/substrate
mechanism. The results are in accordance to several published
works and confirm the hypotheses presented in the literature on
the mechanical behavior of geopolymers [48,50,54].
Initially, it is observed the modulus of elasticity of the geopoly-
mers is able to reach high values with increase of the Si/Al ratio.
For the Si/Al ratio  1.90, the values are very close to each other
and they are independent of the alkaline-activating solution type
[48]. The geopolymeric resins in this study presented Si/Al ratios
between 1.89 and 1.97, as shown in section 2.1.k
Duxson et al. [48] also suggest that geopolymers prepared from
potassium hydroxide have lower modulus of elasticity than those
from sodium hydroxide, for Si/Al ratio between 1.15 and 1.90
and for the same type of silicate used in the mixture. The geopoly-
meric resins of this work produced with mixed alkaline-activating
solutions (sodium and potassium silicates/hydroxides) exhibited
intermediate values of modulus of elasticity.
The Poisson’s ratio of the geopolymeric resins in this study are
close to those reported by Hardjito et al. [55]. Table 8 shows that
the geopolymeric resins activated by sodium hydroxide presented
slightly higher values than those activated by potassium hydrox-
ide. Likewise, Rocha et al. [8] obtained values of Poisson’s ratio
between 0.20 and 0.24 for geopolymeric mortars activated by

Table 7
Indirect tensile strength values of metakaolin-based geopolymeric resins at 28 days.

Geopolymeric resin Tensile strength at 28 days (MPa)

Present work Rocha et al. (2018) Nguyen (2005) NBR 6118 (2014)
S.s – S.h 5.80 ± 0.08 5.20 ± 0.70 5.33 4.97
S.s – P.h 5.75 ± 0.05 4.10 ± 0.30 5.23 4.89
P.s – S.h 6.03 ± 0.05 4.90 ± 0.60 5.32 4.97
P.s – P.h 5.77 ± 0.21 4.00 ± 0.30 5.19 4.41

7
Joadelio Chagas Soares, Dylmar Penteado Dias, Eduardo Atem de Carvalho et al. Construction and Building Materials 275 (2021) 122120

Fig. 9. Rupture of geopolymeric resin in: (a) compressive testing; (b) indirect tensile testing.

Table 8
The shear strength (s12) and shear modulus (G12) for the
Compressive strength, longitudinal elastic modulus and Poisson’s ratio of metakaolin-
based geopolymeric resins at 28 days. geopolymeric resins varied from 4.31 to 7.55 MPa and 3.40–8.20
GPa, respectively. The shear modulus values of S.s – P.h and P.s –
Geopolymeric Compressive strength Modulus of elasticity Poisson’s
S.h resins were 36%–141% higher than S.s – S.h and P.s – P.h resins
resin at 28 days (MPa) at 28 days (GPa) ratio
and 91%–156% higher compared to commercial epoxy. S.s – P.h and
S.s – S.h 85.86 ± 0.26 17.86 ± 0.03 0.21
P.s – S.h resins achieved higher values of s12 and G12. They have
S.s – P.h 82.23 ± 0.86 15.30 ± 0.10 0.17
P.s – S.h 85.81 ± 4.78 13.86 ± 0.04 0.18 denser and more homogeneous microstructure, as shown in item
P.s – P.h 80.76 ± 1.28 11.68 ± 0.09 0.17 3.7. Table 9 shows that the values of the shear modulus obtained
in the experimental program are higher than those calculated the-
oretically, since the latter only take into account mechanical
sodium hydroxide and values between 0.13 and 0.17 for those parameters. The shear strength and shear modulus values of com-
potassium hydroxide activation. mercial epoxy resin were 17.88 MPa and 3.20 GPa, respectively.
The commercial epoxy resin reached higher levels of strain and,
consequently, relatively lower values of shear modulus in relation
3.6. Shear strength
to geopolymeric resins.
Studies caring out with different types of epoxy resins found
Fig. 10 compares the shear strength curves of geopolymeric
shear modulus values varying from 1.4 to 5.0 GPa [25,56]. How-
resins to a commercial epoxy resin as function of shear strain. A
ever, studies on shear properties by Iosipescu method are com-
linear trendline was adopted because it better represents the dis-
monly about polymeric matrix composites [59,60]. Gonçalves
persion of results.
et al. [25] used epoxy resins reinforced with glass and carbon fibers
The curves presented similar behavior and trend as reported in
and obtained shear modulus values equal to 7.7 and 35 GPa,
the literature [22,23,56–58]. In the initial phase of the tests, lower
respectively. The shear behavior of cement matrix composites rein-
loads led to negligible strains (less than 200 le). Then, when the
forced with 2% polyvinyl alcohol fibers (PVA) was investigated by
loads reached approximately 25% of shear strength, the curves
Baghi et al. [61], who obtained a value of approximately 4 MPa
showed a linear behavior. The magnitude of stresses and strains
for maximum shear strength with deformation of 500 le.
increased significantly until the appearance of first cracks in the
The analysis of the loading data in relation to the strain revealed
notch region. Finally, the specimens reached maximum bearing
that the specimens ruptured by shear, which indicated by the
capacity and failed abruptly with the increase and propagation of
abrupt drop in the loading process. ASTM D 5379 [23] specifies
cracks.
typical acceptable fracture patterns for the Iosipescu method.
The geopolymeric resins showed strain values of about 1000 to
Fig. 11 shows this fracture pattern, for both geopolymeric resins
2000 le for the maximum shear strength. The commercial epoxy
and commercial epoxy one. This type of rupture occurred in the
resin achieved greater strain, approximately 9000 le. It is worth
notch region before the local crushing in the loading line, which
mentioning that during the Iosipescu test some specimens showed
is a common behavior for isotropic materials and composites with
atypical behavior and were discarded.
good fiber–matrix adherence.
Shear strength and elastic shear modulus were calculated fol-
lowing the ASTM D5379 [23] and the results are shown in Table 9.
The ones obtained in the experimental program for shear modulus 3.7. SEM analysis
were compared to those obtained by the classic definition of G,
according to Eq. (7) proposed by NBR 8522 standard [33]. The micrographs of the Figs. 12 and 13 show the four
metakaolin-based geopolymeric resins with magnifications of
G ¼ Ec=2ð1 þ v Þ ð7Þ 40 and 700, succeeding Iosipescu testing. The morphological
analysis of the fracture surface took into account the homogeneity,
where Ec is the modulus of elasticity and m is the Poisson’s ratio. porosity and microcracks of the matrix and the transition zone of
8
Joadelio Chagas Soares, Dylmar Penteado Dias, Eduardo Atem de Carvalho et al. Construction and Building Materials 275 (2021) 122120

Fig. 10. Curves shear strength versus shear strain in the Iosipescu test: (a) S.s – S.h; (b) S.s – P.h; (c) P.s – S.h; (d) P.s – P.h; (e) commercial epoxy resin.

and P.s - P.h (activated by potassium hydroxide), which presented

uniform fracture surfaces and with less microcracks. The spherical
Table 9
Shear strength and shear elastic modulus of metakaolin-based geopolymeric resins at
voids occur due to the trapping of air bubbles during molding.
28 days. Microcracks are attributed to the fracture process during mechan-
ical test execution. The massive structure observed in the micro-
Resin type s12 (MPa) G12 (GPa) G (GPa)
NBR 8522 (ABNT, 2017)
graphs confirms the amorphous characteristic of geopolymeric
materials [8,48]. The matrix-fine aggregate transition zone shows
S.s – S.h 4.31 ± 0.47 4.50 7.40
S.s – P.h 7.55 ± 1.58 6.13 6.53
a different behavior among the four geopolymeric resins after fail-
P.s – S.h 6.97 ± 0.79 8.20 5.88 ure. It is possible to notice that S.s - S.h and P.s - P.h resins showed
P.s – P.h 6.84 ± 0.62 3.40 4.98 more cracks in the transition zone (surrounding the fine aggregate)
Commercial epoxy 17.88 ± 1.89 3.20 1.30 compared to S.s - P.h and P.s - S.h. In Fig. 14a, the commercial
epoxy resin matrix proved to be quite resistant, despite the pres-
ence of numerous pores, and the transition zone indicates excellent
adherence between the matrix and the fine aggregate. However, it
matrix-fine aggregate. The geopolymeric resins presented homoge- is possible to observe a generalized microcracking development in
neous matrices and dense gel phase, mainly consisting of S.s - P.h the epoxy resin matrix. The commercial epoxy resin matrix also

9
Joadelio Chagas Soares, Dylmar Penteado Dias, Eduardo Atem de Carvalho et al.
Fig. 11. Rupture mode of specimens in the Iosipescu test: (a) geopolymeric resin; (b) commercial epoxy resin.
Fig. 12. SEM images of geopolymeric resins produced with alkaline sodium silicate: (a) S.s – S.h (40); (b) S.s – S.h (700); (c) S.s – P.h (40), (d) S.s – P.h (700).
showed a denser transition zone, surrounding the fine aggregate
(Fig. 14b).
4. Conclusions
The analysis of the results obtained in the experimental pro-
gram for the four metakaolin-based geopolymeric resins activated
by different combinations of silicates and hydroxides in compar-
ison to a commercial epoxy resin concludes that:
(1) the presence of KOH in the alkaline-activating solution
improved resin workability since the solutions with KOH
were less viscous than those with NaOH for the same
silicate;
(2) the high presence of sodium cations in the composition of
alkaline-activating solutions reduced initial and final setting
times, confirming their influence on these parameters;
10
Construction and Building Materials 275 (2021) 122120
(3) the adhesion coefficients between substrate/geopolymer
resin interfaces were satisfactory and comparable to other
well-known materials used in structural repairs (e.g. epoxy
resin and polymeric mortars, etc.);
(4) all geopolymeric resins showed compressive strength above
80 MPa at 28 days of age, especially in the early ages due to
quick geopolymerization. The indirect tensile strength of
geopolymeric resins showed an average of 7% in relation to
the compressive strength;
(5) the moduli of elasticity of the geopolymeric resins were sim-
ilar to those found in the literature, confirming that this
mechanical property is significantly influenced by the char-
acteristics of the geopolymeric microstructure, which results
from the combination of silicates and hydroxides used in the
alkaline-activating solution;
(6) geopolymeric resins showed good results for shear strength
and shear modulus by Iosipescu test. The resins S.s - P.h and
P.s - S.h presented superior results compared to the other
Joadelio Chagas Soares, Dylmar Penteado Dias, Eduardo Atem de Carvalho et al. Construction and Building Materials 275 (2021) 122120

Fig. 13. SEM images of geopolymeric resins produced with potassium silicate: (a) P.s – S.h (40); (b) P.s – S.h (700); (c) P.s – P.h (40), (d) P.s – P.h (700).

Fig. 14. SEM images of commercial epoxy resin: (a) 40; (b) 700.

ones, which reached values close to 7 MPa for shear strength (9) the geopolymeric resins developed in this work presented a
and between 6.13 and 8.20 GPa for the shear modulus. The satisfactory performance and show high potential for use in
commercial epoxy resin reached a lower average value com- reinforced concrete structure repairing.
pared to the geopolymeric resins produced;
(7) in spite of the metakaolin-based geopolymeric resins having
small differences in composition, alkaline-activating solu-
CRediT authorship contribution statement
tion molar ratios, microstructure and mechanical properties,
they all exhibited the same failure mode by Iosipescu test, as
Joadelio Chagas Soares: Conceptualization, Methodology,
well as the commercial epoxy resin;
Investigation, Writing - original draft, Visualization. Dylmar Pen-
(8) Scanning electron microscopy analysis of fracture surfaces
teado Dias: Supervision, Visualization, Writing - review & editing.
revealed significant differences depending on the type of
Eduardo Atem de Carvalho: Validation, Data curation, Writing -
alkaline-activating solution used. The resins produced with
review & editing. Jodimar Soares de Azevedo: Validation,
potassium hydroxide showed a slightly denser and more
Investigation.
homogeneous matrix, whereas the resins with mixed sili-
cates and hydroxides displayed a transition zone (matrix-
fine aggregate interface) with less cracks than the others.
On the other hand, the commercial epoxy resin showed good Declaration of competing interest
results of mechanical strength, even though the matrix was
quite porous; No conflicts of interest to this work.
11
Joadelio Chagas Soares, Dylmar Penteado Dias, Eduardo Atem de Carvalho et al. Construction and Building Materials 275 (2021) 122120

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