Construction and Building Materials 258 (2020) 119697

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Construction and Building Materials

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

Optimization of a reinforced geopolymer composite using natural fibers

and construction wastes
Guido Silva a, Suyeon Kim a, Bruno Bertolotti b, Javier Nakamatsu c, Rafael Aguilar a,⇑
a
Engineering Department, Pontificia Universidad Catolica del Peru PUCP, Lima, Peru
b
Science Department, Pontificia Universidad Catolica del Peru PUCP, Lima, Peru
c
Research and Development Department, Compañia Minera Agregados Calcareos S.A (COMACSA), Lima, Peru

h i g h l i g h t s

Geopolymer composites from construction wastes and natural fibers were produced.

Good compatibility between the natural fibers and geopolymer matrix was verified.

The fibers significantly increased the mechanical properties of the composites.

The fiber type and aspect ratios defined workability limits and mechanical properties.

Fibers controlled the post peak behavior of the composites in flexure and tension.

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

Article history: Geopolymer technology has allowed the development of eco-friendly construction materials with high
Received 24 December 2019 mechanical properties using industrial wastes and residues. However, geopolymers show fragility and
Received in revised form 20 May 2020 low ductility behavior similar to Portland cement-based materials. This article focuses on the evaluation
Accepted 22 May 2020
of jute and sisal fibers as reinforcement of a geopolymer matrix produced from residues of Fired Clay
Available online 13 June 2020
Brick Powder (FCBP). Control samples with no fibers and reinforced matrices with different contents of
jute (ranging from 0.5 to 2.0 wt%) and sisal fibers (ranging from 0.5 to 3.0 wt%) were produced to study
Keywords:
the effect of the fiber type and content on the mechanical properties of the resulting geopolymer com-
Sisal fibers
Jute fibers
posites. Mechanical characterization consisted of compression, splitting tensile, and three-point bending
Fired clay brick powder tests. The results of compression and splitting tensile tests showed the existence of an optimum fiber
Geopolymer composite content that depends on the fiber type for reaching the maximum strength while the three-point bending
Short fiber reinforcement test results indicated a linear relationship between the flexural strength and the fiber content. The addi-
Mechanical characterization tion of 2.5% (wt%) of sisal fibers increased the compressive, splitting tensile and flexural strengths up to
76%, 112%, and 270%, respectively, in comparison to the control samples. On the other hand, FCBP-based
geopolymers with 1.5% (wt%) jute fiber reinforcement showed an increase up to 64%, 45%, and 222% of the
compressive, splitting tensile and flexural strengths, respectively. Both, jute and sisal fiber addition at the
optimum content, lead to a change in the failure mode of the samples from a brittle to a more ductile
failure in all mechanical tests.
Ó 2020 Elsevier Ltd. All rights reserved.

1. Introduction higher mechanical properties than Ordinary Portland Cement

Several authors have reported the production of geopolymer
matrices from waste residues and industrial by-products (i.e. fly
ash, ground granulated furnace slag, mine tailings and construction
and demolition wastes, among others) which may even have
⇑ Corresponding author at: Engineering Department, Pontificia Universidad
Catolica del Peru (PUCP), Av. Universitaria 1801, San Miguel, Lima, Peru.
E-mail address: raguilar@pucp.edu.pe (R. Aguilar).
(OPC)-based materials [1–4]. For instance, Atis et al. [1] developed
a geopolymer mortar made from fly ash that reached a compres-
sive strength of up to 120 MPa after only 1 day of being produced.
Cheng and Chiu [2] produced a geopolymer matrix with a 1st-day
compressive strength of 70 MPa using ground granulated furnace
slag. Pacheco-Torgal and Jalili [5] reported the production of tung-
sten mine tailing-based geopolymers with a 28th-day compressive
strength of 40 MPa. High strength geopolymers were also produced
with industrial minerals such as metakaolin [6] reaching a 7th-day

https://doi.org/10.1016/j.conbuildmat.2020.119697
0950-0618/Ó 2020 Elsevier Ltd. All rights reserved.
2 G. Silva et al. / Construction and Building Materials 258 (2020) 119697
compressive strength of 98 MPa, and pozzolan [7] with a 28th-day
compressive strength of 63 MPa. Unfortunately, as other cementi-
tious materials, geopolymer matrices present low tensile strengths
and exhibit a brittle behavior [8].
As for cementitious materials, reinforcement with natural and
synthetic fibers have been proposed as an option to improve duc-
tility and to enhance the performance of geopolymers under ten-
sile stresses. According to Arisoy and Wu [9], the random
addition of short fibers to a cementitious matrix increases its
toughness by providing energy absorption mechanisms, ductility
by allowing multi-cracking, and strength by transferring stresses
across cracks. Most of the research regarding fiber-reinforced
geopolymers have been performed with synthetic fibers such as
steel fibers [10], carbon fibers, glass fibers [11], polypropylene
fibers [12], polyvinyl alcohol fibers [8,13], and basalt fibers
[14,15]. The reinforcement of geopolymer matrices with natural
fibers has received more attention in recent years due to an
increasing environmental concern for finding new energy-
efficient materials with low carbon dioxide (CO2) emissions
[16,17]. In this matter, Correia et al. [18] explored the use of sisal
and pineapple leaf fibers to reinforce metakaolin-based geopoly-
mers. Although they found that a fiber content of 3% (w/v %) had
a negative influence on the compressive strength, the splitting ten-
sile and flexural strengths were significantly improved when com-
pared to the unreinforced matrix. Sisal fibers improved the flexural
and splitting tensile strength by 100% and 111%, respectively,
while pineapple leaf fibers increased them by 43% and 100%,
respectively, in comparison to the strengths of the unreinforced
matrices. Sá et al. [19] were also able to improve the mechanical
properties of metakaolin-based geopolymers by using other natu-
ral fibers. In their study, 5% (wt%) of water and alkali-treated bam-
boo fibers and strips were added to a composite material with
enhanced flexural strength (up to 454% higher than the control
sample). However, similarly to the results obtained by Correia
et al. [18] for pineapple leaf fibers, the compressive strength
decreased by about 50% due to the presence of fibers when com-
pared to the control matrix. Korniejenko et al. [20] explored the
use of cotton, sisal, raffia and coir fibers at 1% (wt%) in fly-ash
based geopolymer composites and evaluated the resultant com-
pressive and flexural strengths. The results indicated that coir, sisal
and cotton fibers increased the compressive strength in up to 27%
when compared to the unreinforced matrix. On the contrary, the
addition of raffia fibers resulted in geopolymer composites with
lower compressive strengths. They also noted that the flexural
strength was not influenced by the presence of coir, sisal and cot-
ton fibers, however, the presence of raffia fibers led to a 45%
decrease in flexural strength. Chen et al. [21] evaluated the effect
of the content of alkali-treated sweet sorghum fibers on the
mechanical properties of fly ash-based geopolymers. They found
an optimum fiber content of 2% (wt%) that caused the highest
splitting tensile and flexural strengths (up to 39% and 36% higher,
respectively, when compared to the control matrix). However, they
also observed a loss of the compressive strength in the resulting
geopolymer composites when the fiber content was increased.
Alomayri et al. [22] also determined an optimum cotton fiber
content (0.5% wt%) that maximized the flexural strength, flexural
modulus and fracture toughness of fly ash-based geopolymer
composites.
As shown by Silva et al. [23], studies of natural fiber reinforce-
ment in geopolymer composites have been mainly focused on
metakaolin and fly ash-based geopolymers. However, high com-
pressive strengths have also been achieved in geopolymer matrices
produced from other sources, such as construction wastes. Komnit-
sas et al. [24] reported the production of geopolymer matrices from
fired clay brick wastes with a 7th-day compressive strength up to
49.5 MPa, while Rakhimova and Rakhimov [25] produced a hybrid
geopolymer mortar with a 28th-day compressive strength of
120 MPa.
From an environmental point of view, fired clay brick wastes
are a perfect candidate as raw materials for the development of
eco-friendly building composites considering the large amounts
of these wastes that are produced around the world. In this respect,
the European Union alone produces around 855 million tons per
year of construction and demolition wastes [26], an average of
30% of this is estimated to be fired clay brick residues [27]. The
development of new construction materials using these residues
together with natural fibers (i.e. cellulosic fibers) is an attractive
alternative for the replacement of traditional OPC-based materials
considering also that it has been reported that natural fibers
exposed to highly alkaline conditions may result in enhanced com-
posite materials properties [28]. In this regard, the objective of this
study was to evaluate the incorporation of natural cellulosic fibers
(specifically, sisal and jute) in the formulation of geopolymers
derived from fired clay brick powder (FCBP) and to analyze possi-
ble negative effects for the resultant mechanical properties due to
the exposition of the fibers to highly alkaline environments at very
early ages and long oven-curing periods. A comprehensive experi-
mental characterization campaign was carried out for this purpose,
it included the evaluation of the optimum quantity of fibers con-
sidering the workability of the mixture and the analysis of the
response of the matrices under compression, splitting and flexural
loading conditions after 7 days of production.
2. Materials and experimental plan
2.1. Materials
Jute fibers are extracted from Corchorus capsularis and Corchorus
olitorius, while sisal fibers are obtained from Agave sisalana. Both
natural fibers are mainly composed of cellulose, hemicellulose,
and lignin, but in different proportions. Jute and sisal fibers were
selected for the present study because they are considered as
future fibers by the Food and Agriculture Organization of the Uni-
ted Nations (FAO) due to the benefits they cause to the environ-
ment. It is estimated that a hectare of jute plants consumes
about 15 tons of CO2 and releases 11 tons of oxygen. On the other
hand, sisal crops absorb more CO2 than they produce, and the
organic wastes produced during sisal fiber production can be
employed in industries such as bioenergy generation, animal feed
and fertilizer production [29]. It has been reported that jute fibers
are composed of 58–63% cellulose, 20–24% hemicellulose, and 12–
15% lignin by weight [30], while sisal fibers contain 43–56% cellu-
lose, 21–24% hemicellulose and 7–9% lignin by weight [31]. Jute
fibers have a density of about 1.30–1.45 g/cm3 while for sisal fibers,
their density is around 1.45 g/cm3 [32]. For the present study, both
fibers were obtained from commercial products (ropes) and cut to
a length of 10 mm, resulting in aspect ratios (l/d) of 189 and 73,
respectively. The cross-sectional and longitudinal morphologies
of both fibers were analyzed by Scanning Electron Microscopy
(SEM) and the results are presented in Fig. 1. Longitudinal micro-
graphs indicate that sisal fibers present rougher surfaces than jute
fibers (see Fig. 1a and b) that can lead to a better adherence
between the fiber and the geopolymer matrix. Fig. 1c and d show
that both fibers are composed of several fiber cells held together
by lignin, a resin-like material [33]. The average diameters of jute
and sisal fibers were calculated as 53 and 137 mm, respectively,
which were measured with a Mitutoyo dial thickness gauge (model
7301).
Sisal and jute fibers were subjected to water absorption and
water contact angle tests to investigate the wettability of the
fibers. Both fibers were dried out at 65 °C for 24 h before the tests.
 G. Silva et al. / Construction and Building Materials 258 (2020) 119697
Fig. 1. SEM micrographs of natural fibers used as reinforcement of FCBP-based geopolymer matrices: (a) Longitudinal view of jute fibers; (b) Longitudinal view of sisal fibers;
(c) Cross-sectional view of jute fibers; (d) Cross-sectional view of sisal fibers.
For water absorption tests, the fibers were immersed in water for
24 h after being dried. Then, the excess of water was removed from
the surface of the fibers with absorbent paper which allowed them
to reach a saturated surface dry condition (SSD). The water absorp-
tion capacity (A) was calculated using Equation (1) where W and D
are the weights at the SSD and dry conditions of the fibers,
respectively.
W D
WaterabsorptionðAÞ; % ¼ ½   100 ð1Þ
D under uniaxial tensile loads, Fig. 3a shows the results of the tensile
On the other hand, for contact angle tests, a series of fibers were
aligned and packed together forming a flat surface about 1.5 mm
wide on a glass slide. A single droplet of distilled water (0.5 mL)
was applied on the surface of the flattened group of fibers and
the contact angle was measured using a Ramé-hart contact angle
goniometer after 1, 10, 20, and 30 s.
The results of the water absorption tests gave values of 125% ±
5% and 102% ± 13% for sisal and jute fibers, respectively, which
indicates that sisal has a better water absorption capacity than jute
fibers. Water contact angle tests (Fig. 2) also indicate that sisal
fibers are significantly more hydrophillic than jute fibers. Jute
fibers showed a contact angle of 70° even after 30 s of exposure
to the water droplet. On the contrary, sisal fibers exhibited a lower
initial contact angle of 45° after 1 s of exposure which rapidly
decreased. Ten seconds after setting the water drop, no contact
angle could be measured because the drop had been absorbed by
the material (Fig. 2j). These results indicate that sisal fibers have
better affinity to water than jute fibers, this is critical for the for-
mation of a good and stronger interaction between the fiber and
the geopolymer matrix, which is a water-based material [34].
3
The tensile strengths of jute and sisal fibers were investigated
through direct tensile tests carried out in an MTS Exceed 42.503
machine with 5 kN capacity at a displacement rate of 6 mm/min.
Single fiber tensile tests were performed following the guidelines
of ASTM D3822 [35]. Tensile stresses were calculated as the ratio
of the applied load and the average transversal area of the fiber.
The ratio between the crosshead displacements and the distance
between grips were taken as the strain to develop the tensile stress
vs strain curves. Six specimens of each type of fiber were tested
strength tests for both fibers. As shown, sisal fibers have more ten-
sile strength than jute fibers; the tensile strength of sisal fibers was
508 MPa, while the strength of jute fibers was 276 MPa. The tensile
stress vs. strain curves of both fibers is presented in Fig. 3b. It can
be observed that despite the difference in their tensile strengths,
both fibers have a similar modulus of elasticity (E-modulus). The
value for the E-modulus for jute fibers was 27 GPa while sisal pre-
sented a slightly lower value of 25 GPa. However, sisal fibers pre-
sented 97% more elongation capacity than jute fibers as is shown
in Fig. 3b.
Milled fired clay bricks (here on named as fired clay brick pow-
der – FCBP) from construction wastes in Lima (Peru) were used as
source material for the production of geopolymer composites. After
the samples were collected, they were milled in a process that con-
sisted of three phases: brick particles passed through i) an impact
crusher, ii) a rolling mill, and iii) a ball mill. The particle size distri-
bution of the raw material was determined using a particle size
analyzer, Sedigraph 5100, which works based on the sedimenta-
tion technique and X-ray photon absorption. Particle size distribu-
tion analysis of milled FCBP resulted in a mean particle size of
4 G. Silva et al. / Construction and Building Materials 258 (2020) 119697

(a) (b) (c) (d)

(e) (f) (g) (h)

90 90
80 80

Water contact angle ( °)

Water contact angle ( °)

70 70
60 60

Not determinable

Not determinable

Not determinable
50 50
40 40
30 30
20 20
10 10
0 0
1 10 20 30 1 10 20 30
Time (s) Time (s)
(i) (j)
Fig. 2. Water contact angle tests on fibers: (a-d) jute fibers at 1, 10, 20, and 30 s; (e-h) sisal fibers at 1, 10, 20, 30 s; (i) time variation in jute fibers and (j) time variation in sisal
fibers.

600 600
Jute
Tensile strength (MPa)

500
Tensile stress (MPa)

500
400 400
300 300
200 200

100 100

0 0
Jute Sisal 0 0.01 0.02 0.03
Fiber type Strain (mm/mm)
(a) (b)

Fig. 3. Tensile test of single jute and sisal fibers: (a) Tensile strengths; (b) Tensile stress vs strain curves.

17.14 um (Fig. 4a) which may favor the reactivity of the raw mate- 2.2. Experimental procedures
rial. The SEM micrograph presented in Fig. 4b shows a very irreg-
ular and crystal-like shape morphology for FCBP. Fresh FCBP-based geopolymer composites were subjected to
X-ray fluorescence analysis of the FCBP showed a chemical flow tests according to ASTM C1437-15 [37] to study the influ-
composition (see Table 1) with a high content of SiO2, Al2O3 and ence of the amount of jute and sisal fibers on the workability
Fe2O3 which confirms the appropriate condition for the production of the mixture. For this purpose, the fresh material was poured
of geopolymers. More information regarding the chemical, physi- into a truncated conical mold (70 mm top diameter, 100 mm
cal, mineralogical and microscopic analysis of the FCBP used in this bottom diameter and 50 mm height) in two equal layers and
work can be found in ref. [36]. was compacted by tamping each layer 20 times (one test per
The alkaline activating solution was prepared by mixing NaOH series). After 1 min of material setting, the mold was removed
pearls (99% wt., purity), a sodium silicate solution and distilled and the flow table was dropped 25 times in 15 s and four mea-
water. The chemical composition of the sodium silicate solution surements of the base diameter of the resultant mass were
was SiO2 28%, Na2O 8%, and H2O 64%, by weight. recorded.

100
Cumulative Finer Mass (%)
80
60
40
20
0
100
Fig. 4. Particle size distribution and morphology of FCBP: (a) Granulometric curves envelope and (b) SEM micrograph.
Table 1
Chemical composition of FCBP by X-ray fluorescence spectroscopy.
Oxide content (w/w, %)
SiO2 Al2O3
53.45 20.52
Bulk density measurements were also carried out in all samples
to investigate its relationship with the flow measurements and the
mechanical properties of the fiber-reinforced geopolymer compos-
ites. Determination of bulk density (Db) was carried out by using
the following equation:
M
Db ¼
V
where Db = bulk density, M = mass of the tested specimen, and
V = volume of the sample.
To evaluate the influence of the addition of jute and sisal fibers
in the mechanical properties of FCBP-based geopolymer compos-
ites, uniaxial compression tests, splitting test, and three-point
bending tests were performed according to procedures described
in ASTM C109 [38], ASTM C496 [39] and ASTM C348 [40], respec-
tively. An electromechanical testing machine MTS Exceed 45.105
(Fig. 5a) with 100 kN capacity was used for all mechanical tests
of geopolymer composites. The displacement rate of the load frame
was set at 0.5 mm/min and the global displacements correspond-
ing to the displacements of the load frame were recorded for all
the mechanical tests. 50 mm-side cubic samples were used for
compression tests (see Fig. 5b), cylindrical specimens (40 mm
diameter and 80 mm height) were used for splitting tests (see
Fig. 5c), while three-point bending tests involved prismatic sam-
ples with approximate dimensions of 40 mm  40 mm (cross-sec
tion)  160 mm (length) (Fig. 5d). SEM was used to study the dis-
tribution and interaction of jute and sisal fibers within the binder
mixture. A FEI Quanta 200 SEM performed all SEM imaging of
fiber-reinforced broken samples with an operating voltage of
30 kV.
2.3. Preparation of samples
Unreinforced geopolymer matrices (control matrices) and Fiber
Reinforced Geopolymer Composites (FRGC) were prepared to study
their effect on the mechanical properties. FCBP and natural fibers
were dry-mixed to ensure homogenous distribution. After that,
the alkaline activating solution was gradually added and mixed
until a homogenous paste was obtained with the aid of a mortar
G. Silva et al. / Construction and Building Materials 258 (2020) 119697 5
10 1 100 μm
Particle size (μm)
(a ) (b)
Fe2O3 K2O MgO CaO Na2O Others
7.80 2.63 1.85 1.62 1.50 10.63
mixing machine type STJBJ-5 (see details for the optimization of
the activating solution in ref. [36]). As shown in Fig. 6, optical
microscope images of the different matrices show a proper distri-
bution of fibers after the mixing process.
Different contents of jute and sisal fibers in the reinforced com-
posites were studied. The evaluated compositions varied from 0.5%
ð3Þ to 2% (wt%) of jute fibers in the FRGC and 0.5% to 3% (wt%) of sisal
fibers in the FRGC. The maximum amount of fibers was limited by
the workability of the mixture to avoid poor casting conditions
caused by difficulties in filling, vibrating and compacting the mix-
ture. The addition of more water to counterbalance the loss of
workability due to the presence of fibers was not considered since
data from other studies showed that the addition of extra water
decreased the mechanical properties of geopolymer matrices
[41]. Cubic, cylindrical and prismatic silicon molds were filled with
the geopolymer mixtures and were then subjected to vibration to
remove trapped air bubbles. Specimens were cured in an oven at
65 °C for 3 days (samples were de-molded after 24 h, but kept in
the oven) and then left at room temperature for four more days
until mechanical tests were conducted. The oven curing time was
limited to 3 days to avoid the degradation of the fibers in FRGC.
As demonstrated by the authors in [36], curing at ambient temper-
ature was disregarded as the FCBP-based geopolymers need rela-
tively high temperatures in the initial phase to form. Table 2
presents a summary of the preparation and curing conditions of
the FRGCs, as well as the number of tested samples in the mechan-
ical tests.
3. Results and discussion
3.1. Fresh properties of fiber-reinforced geopolymer composites
Fig. 7 shows the influence of jute and sisal fibers incorporation
on the workability (measured by the flowability of the mixtures) of
geopolymer composites. The flowability (F) was measured using
Eq. (2) as the relative difference of the average base diameter of
the tested matrix (D) with respect to the mold bottom diameter
(Do).
6 G. Silva et al. / Construction and Building Materials 258 (2020) 119697

50
50 50

(b)

Geopolymer
sample

40
80

40 (c)

160
40
120
(a) ( d)
Fig. 5. Mechanical characterization: (a) Universal testing machine used in mechanical characterization of geopolymer composites; (b) Geopolymer composite cubic sample
and compression test; (c) Geopolymer composite cylindrical sample and splitting tensile test; (d) Geopolymer composite prismatic sample and three-point bending test.
(Units in mm).

600 μm 600 μm 600 μm

(a) (b) (c)

Fig. 6. Optical microscope images of fresh geopolymer composites: (a) Control matrix; (b) Jute-FRGC (1.5% wt. fiber content); and (c) Sisal-FRGC (2.5% wt. fiber content).

Table 2
Summary of preparation and curing conditions of the FRGCs (the # of tested samples include the number of samples tested in uniaxial compression, splitting tensile and flexural
tests).

Fiber type Fiber addition # of tested samples Ms (mol/mol) Na2O Water/binder Oven curing temperature and time Total curing time
(wt%) (in mechanical tests) (wt%) (wt./wt.)
Control matrix – 9 0.60 8 0.27 3 d at 65 °C 7d
Jute 0.50 9 0.60 8 0.27 3 d at 65 °C 7d
1.00 9
1.50 9
2.00 9
Sisal 0.50 9 0.60 8 0.27 3 d at 65 °C 7d
1.00 9
1.50 9
2.00 9
2.50 9
3.00 9
 G. Silva et al. / Construction and Building Materials 258 (2020) 119697 7

150
Jute FRG Sisal FRG
D
100

Flow (%)
50

0
Control 0.5 1.0 1.5 2.0 2.5 3.0
Fiber addition (%)
(a) (b)
Fig. 7. Flow tests in FRGSs: (a) Flow test set up; (b) Results of flowability tests in matrices reinforced with jute and sisal fibers.

 
D  D0 research no extra water was added to recover the loss of workabil-
F¼ 100 ð2Þ
D0 ity when fibers were added. An eventual addition of extra water to
the mixture and its subsequent evaporation during curing would
The results presented in Fig. 7b indicate the existence of an indi-
cause the formation of large quantities of intergranular pores in
rect relationship between the flowability of both FRGCs and their
the microstructure that would lead to a decrease in the bulk den-
fiber content. However, for equal fiber content, sisal-FRGCs evi-
sity of the composites [22]. The initial gain of density seen in both
denced a lower reduction in workability. For example, for a fiber
FRGCs compared to the control matrix can be explained by higher
content of 2%, sisal-FRGC evidenced a flow capacity 50% higher
compaction used during manufacturing due to the loss of worka-
than that of jute-FRGC. This can be attributed to the lower aspect
bility and increase of the viscosity of the fresh mixtures due to fiber
ratio presented by sisal fibers as reported by Yazici et al. [42]
addition. However, more than 1% (wt.) of fibers produces a
who stated that the workability of fiber-reinforced cementitious
decrease of the bulk density in both FRGCs. The reason for this loss
materials decreases as the aspect ratio increases. This test allowed
in bulk density, even when higher compaction energy was
the definition of the maximum amount of jute (2%) and sisal fibers
employed during manufacturing, may be because fiber agglomera-
(3%) that could be incorporated in the mixtures. A higher amount
tion during mixing occurs with high fiber contents. Agglomeration
of fiber was not possible to evaluate since the casting processes
of fibers in composites produce intergranular pores which may
became extremely difficult.
have also negative effects on the mechanical properties of the com-
posites [22].
3.2. Hardened properties of fiber-reinforced geopolymer composites

3.2.1. Bulk density 3.2.2. Compression strength

Fig. 8a and b show the bulk density results of FRGCs reinforced Fig. 9 shows the results of the uniaxial compression tests per-
with jute and sisal fibers, respectively. Unlike other studies that formed in the control samples and the FRGCs. As shown in
report an inversely proportional relationship between the bulk Fig. 9a and b, the compressive strengths of both geopolymer com-
density and the fiber content [22,34,43], Fig. 8 shows that there posites exhibit an improved behavior when compared to the con-
is a specific value of fiber content that maximizes the bulk density trol sample. Moreover, the results indicate a trend, an increase in
(1% for both sisal-FRGC and jute-FRGC). This notable difference the strength with more fiber content, up to a limit where a
with other reports can be attributed to the fact that in the current decrease is observed, and that the maximum strength depends

2000 2000
Bulk densitty (kg/m3)
Bulk densitty (kg/m3)

1900 1900

1800 1800

1700 1700
Control 0.5 1.0 1.5 2.0 Control 0.5 1.0 1.5 2.0 2.5 3.0
matrix Fiber addition (%) matrix Fiber addition (%)
(a) (b)
Fig. 8. Bulk density test results for fiber-reinforced geopolymer composites: (a) Density of specimens reinforced with jute fibers, and (b) Density of specimens reinforced with
sisal fibers.
8 G. Silva et al. / Construction and Building Materials 258 (2020) 119697

25 25
Optimum condition Optimum condition

Compressive strength (MPa)

Compressive strength (MPa)

20 20

15 15

10 10

5 5

0 0
Control 0.5 1.0 1.5 2.0 Control 0.5 1.0 1.5 2.0 2.5 3.0
matrix matrix
Fiber addition (wt. %) Fiber addition (wt. %)
(a) (b)

30
Control matrix
Jute FRGC - 1.5% (wt.)
Compression stress (MPa)

25
Sisal FRGC - 2.5% (wt.)

20
(d)
15

10

0
0 0.05 0.1
Strain (mm/mm) (e)

(c) (f)
Fig. 9. Compression test results for fiber-reinforced geopolymer composites: (a) 7th-day compressive strengths of specimens reinforced with jute; (b) 7th-day compressive
strengths of specimens reinforced with sisal fibers; (c) Compression vs. strain curves; (d) Failure mode of control matrix; (e) Failure mode of jute-FRGC (1.5% fiber content); (f)
Failure mode of sisal-FRGC (2.5% fiber content).

on the fiber type. In the case of jute-FRGC, the 7th-day compressive tests. Fig. 9d shows the brittle failure mode exhibited by the con-
strength reached a maximum of 20.6 MPa when the content of trol matrix (no fiber-reinforcement), with small free fragments
fibers was 1.5% (wt%), representing an increase of 64% in compar- being produced. On the other hand, the failure modes of FRGCs
ison to the control. On the other hand, sisal-FRGC samples with with jute and sisal fibers clearly show a more ductile behavior
2.5% (wt%) fibers produced the highest improvement (76%) on (Fig. 9e and f).
the 7th-day compressive strength when compared to the control
matrix, reaching 22.1 MPa. Higher fiber contents led to a decrease 3.2.3. Tensile strength
in the compressive strength for both types of FGRC. Jute-FRGC with The results of the splitting tests are shown in Fig. 10. As shown,
more fibers than 1.5% (wt%) showed a lower compressive strength the addition of jute and sisal fibers improved the behavior of the
(19.0 MPa), while sisal-FRGC with 3% (wt%) fibers showed a com- tested matrices under tensile stresses. Similar to what was
pressive strength of 18.0 MPa. The compression stress–strain observed in compression tests, both FRGCs showed an increase in
curves for the control matrix, the optimum jute-FRGC (with a fiber the splitting tensile strength with more fiber content until an opti-
content of 1.5 wt%) and sisal-FRGC (2.5 wt% fiber) are shown in mum value. For jute-FRGCs, the highest splitting tensile strength
Fig. 9c. An increase in the E-modulus can be observed in both jute (1.6 MPa) was obtained with the addition of 1.5% (wt%) of fibers
and sisal-FRGCs compared to the control matrix, 103% for jute and (the same optimum value obtained in the compression tests) sur-
76% for sisal. The presence of both types of fibers changed signifi- passing in 45% the strength of control matrix. In the case of sisal-
cantly the way the samples broke apart during the compression FRGCs, the addition of 2.5% (wt%) of fibers (also the same optimum
 G. Silva et al. / Construction and Building Materials 258 (2020) 119697 9

Splitting tensile strength (MPa)

2.7

Splitting tensile strength (MPa)

2.7 Optimum condition
2.4 2.4
2.1 Optimum condition 2.1
1.8 1.8
1.5 1.5
1.2 1.2
0.9 0.9
0.6 0.6
0.3 0.3
0.0 0.0
Control 0.5 1.0 1.5 2.0 Control 0.5 1.0 1.5 2.0 2.5 3.0
matrix matrix
Fiber addition (wt. %) Fiber addition (wt. %)
(a) (b)

3.0 Control matrix

Splitting tensile stress (MPa)

Jute FRGC - 1.5% (wt.)

2.5 Sisal FRGC - 2.5 (wt.)
(d)
2.0

1.5

1.0

0.5

0.0
0 1 2 3 4
(e)
Displacement (mm)

(c) (f)
Fig. 10. Splitting test results for fiber-reinforced geopolymer composites: (a) 7th-day splitting tensile strengths in specimens reinforced with jute; (b) 7th-day splitting
tensile strengths in specimens reinforced with sisal fibers; (c) Tensile stress vs displacement curves; (d) Failure mode of control matrix; (e) Failure mode of jute-FRGC (1.5%
fiber content); (f) Failure mode of sisal-FRGC (2.5% fiber content).

value obtained in the compression tests) increased the tensile 3.2.4. Flexural strength
strength up to 2.3 MPa (112% higher than the control matrix). The results of the three-point bending tests are presented in
FRGCs with the optimum fiber content also exhibited a better ten- Fig. 11. As shown, the influence of sisal and jute fiber reinforce-
sile toughness in comparison to the control matrix (see Fig. 10c). ment in the flexural response of the resulting geopolymer compos-
The tensile toughness is defined as the area under the splitting ten- ites is evident. Unlike the results of compression and splitting
sile stress vs. displacement curve. 1.5% jute FRGC and 2.5% sisal tensile tests, a linear relationship between the flexural strength
FRGC presented an increment of 92% and 181% in the tensile and the fiber content was observed for both types of FRGCs
toughness, respectively, compared to the control matrix (1.4 (Fig. 11a and b). The flexural strengths of the samples with opti-
kNm1). Finally, the splitting test of FRGCs also showed a more mum fiber content from previous compressive and tensile
ductile failure mode in comparison to the control matrix (see strengths were 2.48 MPa for jute-FRGC (1.5 wt% fiber) and
Fig. 10e and f). The fracture behavior of FRGCs is characterized 2.9 MPa for sisal-FRGC (2.5 wt% fiber), which correspond to an
by multi-cracking since the fibers allow the load transference from increase of 222% and 270%, respectively, in comparison to the flex-
the cracked area to other intact parts of the sample. These results ural strength of the unreinforced FCBP-based geopolymer. How-
are in agreement with what was reported by other authors [8,21] ever, these flexural strengths were not the highest; for the three-
regarding the transition from brittle to ductile behavior of fly ash point bending tests, the maximum flexural strength was achieved
based-geopolymer matrices by the addition of short fibers. with the highest fiber content (limited by the workability and
10 G. Silva et al. / Construction and Building Materials 258 (2020) 119697

4.0 4.0
Optimum condition Optimum condition
3.5 3.5

Flexural strength (MPa)

Flexural strength (MPa)
3.0 3.0
2.5 2.5
2.0 2.0
1.5 1.5
1.0 1.0
0.5 0.5
0.0 0.0
Control 0.5 1.0 1.5 2.0 Control 0.5 1.0 1.5 2.0 2.5 3.0
matrix matrix
Fiber addition (wt. %) Fiber addition (wt. %)

(a) (b)

5.0
Control matrix
4.5 Jute FRGC - 2% (wt.)
Sisal FRGC - 3% (wt.)
Flexural stress (MPa)

4.0
3.5
(d)
3.0
2.5
2.0
1.5
1.0
0.5
(e)
0.0
0 1 2
Displacement (mm)

(c) (f)
Fig. 11. Three-point bending test results of fiber-reinforced geopolymer composites: (a) 7th-day flexural strengths in specimens reinforced with jute; (b) 7th-day flexural
strengths in specimens reinforced with sisal fibers; (c) Flexural stress vs displacement curves; (d) Failure mode of control matrix; (e) Failure mode of jute-FRGC (2% fiber
content); (f) Failure mode of sisal-FRGC (3% fiber content).

homogeneity of the samples). For jute-FRGCs, the highest flexural this respect, a key parameter to understand the mechanical perfor-
strength, 3.3 MPa, was obtained with a fiber content of 2% (wt%), mance of natural fiber reinforced cementitious materials is the
this represents an increase of 329% in comparison to the control structure of the fiber–matrix interface [44,45]. Ardanuy et al. [45]
matrix. On the other hand, the addition of 3% (wt%) sisal fibers to claimed that good interactions between the cement matrix and
the geopolymer matrix produced an increase of 360% of the flexu- natural fibers are crucial to promoting energy absorption mecha-
ral strength compared to the control matrix, reaching 3.5 MPa. It nisms (e.g. fiber debonding, pull-out and stress transfer from the
has been proposed that the improvement of the flexural strength matrix to the fiber). To analyze the fiber–matrix interface in jute
observed in the FRGCs is because the fibers help to carry more ten- and sisal-FRGCs, SEM imaging characterization was performed in
sile loads across cracks, as reported by Sun et al. [8] and Chen et al. 2% jute-FRGC and 3% sisal-FRGC broken samples from three-point
[21]. The failure modes of the control matrix, 2% jute-FRGC and 3% bending tests. SEM images displayed in Fig. 12a and c show a good
sisal-FRGC at the ultimate state are shown in Fig. 11d, 11e, and 11f, adherence between both jute and sisal fibers and the FCBP-based
respectively. It is apparent that the addition of both fibers causes a geopolymer matrix, respectively. Fiber fracture and pull-out from
significant change in the failure behavior, from an abrupt brittle the matrix were identified as the predominant failure mechanisms
crack to a controlled and more cohesive failure, when specimens in both FRGCs (Fig. 12b and d). The good fiber–matrix interaction,
are reinforced with fibers. Even though the response of the control together with the failure mechanisms explains the improved
matrix, 2% jute-FRGC and 3% sisal-FRGC under flexural loads in mechanical behavior of jute and sisal-FRGCs in comparison with
terms of the flexural strength and failure modes is very different, the control matrix seen in all mechanical tests. On the other hand,
the flexural stress vs. displacement curves (Fig. 11c) showed that the decrease in the compressive and splitting tensile strengths
the flexural modulus of the control matrix and FRGCs are roughly observed at the maximum fiber contents (2% jute-FRGC and 3%
similar (~90 MPa). sisal-FRGC) may have been caused by an inefficient compaction
As has been shown, the results of the mechanical tests indicate due to poor workability and a non-uniform microstructure caused
that the structure of the geopolymer matrix and type and content by fiber agglomeration (Fig. 12b), which occurs when higher fiber
of the natural fibers governed the mechanical behavior of FRGCs. In contents are used.
 G. Silva et al. / Construction and Building Materials 258 (2020) 119697
300 μm
(a)
500 μm
(b)
Fig. 12. SEM micrographs of broken FRGCs: (a) Fiber-matrix bonding in jute-FRGC (2% wt%); (b) Failure mechanisms of jute-FRGC (2% wt%); (c) Fiber-matrix bonding in sisal-
FRGC (3% wt%); (d) Failure mechanisms of sisal-FRGC (3% wt%).
4. Conclusions
Natural fiber reinforced fired clay brick powder-based
geopolymer, a potential construction material with good mechan-
ical properties and low environmental impact has been devel-
oped. Short jute and sisal fibers were able to improve the
mechanical behavior of geopolymers made from brick wastes.
The type and amount of fibers mixed with FCBP determine the
fresh and hardened properties of the fiber-reinforced geopolymer
composites. Jute-FRGC with a 1.5% (by weight) fiber content
showed the largest increase in compressive and tensile strengths,
64% and 45%, respectively, in comparison to the control matrix
(unreinforced FCBP-based geopolymer). For sisal-FRGCs, a content
of 2.5% (wt%) fibers showed the best performance increasing the
compressive strength in 76% and the tensile strength in 112%,
when compared to the control matrix. The addition of fibers pro-
moted a more ductile behavior and less brittle rupture of the
reinforced samples which were evident in all the stress–strain
curves and the failure mode of the specimens. Three-point bend-
ing tests showed a linear relationship between the flexural
strength of FRGCs and the natural fiber content. The flexural
strength of jute-FRGC with 2% fiber content was 3.3 MPa, which
corresponds to an increment of 329% in comparison to the unre-
inforced matrix. Similarly, sisal-FRGCs showed the best perfor-
mance with a 3% fiber content showing a flexural strength of
3.5 MPa (a 360% improvement compared to the unreinforced
FCBP-based geopolymer).
11
1 mm
(c)
500 μm
(d)
CRediT authorship contribution statement
Guido Silva: Investigation, Methodology, Writing - review &
editing, Formal analysis. Suyeon Kim: Conceptualization, Investi-
gation, Supervision, Writing - review & editing, Funding acquisi-
tion. Bruno Bertolotti: Investigation, Conceptualization. Javier
Nakamatsu: Conceptualization, Methodology, Investigation,
Supervision, Writing - review & editing. Rafael Aguilar: Conceptu-
alization, Methodology, Investigation, Supervision, Writing -
review & editing, Funding acquisition, Project administration.
Declaration of Competing Interest
The authors declare that they have no known competing finan-
cial interests or personal relationships that could have appeared
to influence the work reported in this paper.
Acknowledgments
This work was supported by CONCYTEC and SENCICO PERU
under the project: ‘‘GeoBloque: Desarrollo de bloques de con-
strucción ultraligeros con geopolímeros” (Contract No. 105-207-
FONDECYT), and by CONCYTEC (J108-2016) under the ERANet-
LAC project (ELAC2015/T02-0721): ‘‘Development of eco-friendly
composite materials based on geopolymer matrix and reinforced
with waste fibers”. The authors are very grateful to Compañía Min-
era Agregados Calcáreos S.A (COMACSA) for providing the use of its
12 G. Silva et al. / Construction and Building Materials 258 (2020) 119697
facilities and equipment. Guido Silva also acknowledges the fel-
lowship from CONCYTEC (contract N° 10-2018-FONDECYT/BM)
for performing his Ph.D. studies.
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