Construction and Building Materials 150 (2017) 817–824

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Construction and Building Materials

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

Influence of various parameters on strength and absorption properties of

fly ash based geopolymer concrete designed by Taguchi method
Ankur Mehta a,⇑, Rafat Siddique a, Bhanu Pratap Singh b, Salima Aggoun c, Grzegorz Łagód d,
Danuta Barnat-Hunek e
a
Department of Civil Engineering, Thapar University, Patiala, India
b
Department of Mechanical Engineering, PEC University of Technology, Chandigarh, India
c
Department of Civil Engineering, University of Cergy Pontoise, France
d
Faculty of Environmental Engineering, Lublin University of Technology, Lublin, Poland
e
Faculty of Civil Engineering and Architecture, Lublin University of Technology, Lublin, Poland

h i g h l i g h t s

Effect of OPC content on properties of geopolymer concrete.

Effect of sodium hydroxide molarity on properties of geopolymer concrete.

Effect of curing temperature on properties of geopolymer concrete.

SEM, EDS and XRD analysis of geopolymer concrete optimized by Taguchi method.

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

Article history: The paper presents the influence of various parameters on compressive strength and water absorption
Received 22 April 2017 properties of fly ash based geopolymer concrete mixtures optimized by Taguchi method. A total of six-
Received in revised form 6 June 2017 teen mixtures were evaluated considering the effect of inclusion of ordinary Portland cement as fly
Accepted 12 June 2017
ash replacement, different molarities of sodium hydroxide solution and different curing temperatures.
Available online 16 June 2017
Analysis of variance was employed to study their influence on compressive strength and water absorp-
tion. Also, using multiple regression analysis, mathematical models were developed for both the proper-
Keywords:
ties followed by their confirmation test results.
Geopolymer
Fly ash
Results show that maximum 7 days compressive strength of 64.39 MPa and minimum water absorp-
Analysis of variance tion of 3.04% was obtained for fly ash based geopolymer concrete with the considered parameters. The
Taguchi method inclusion of additional calcium (in form of OPC as fly ash replacement) was found to influence the com-
Compressive strength pressive strength and water absorption properties most significantly. The best parametric combinations
Water absorption for both the properties were also obtained using Signal-to-Noise ratio graphs. Microstructure properties
were also examined using Scanning Electron Microscopy, Energy Dispersive Spectroscopy and X-ray
Diffraction analysis which confirmed more compact and less permeable matrix for the optimized
mixture.
Ó 2017 Elsevier Ltd. All rights reserved.

1. Introduction be considered as a major problem which is creating the need for

The construction industry is the fastest growing industrial
sector of the world of which Portland cement is the major con-
stituent. However, the release of around 5–7% of total carbon diox-
ide emissions during the production of Portland cement makes
which it highly energy intensive [1]. Today global warming can
⇑ Corresponding author.
E-mail address: ankurmehta07@gmail.com (A. Mehta).
sustainable development in all industrial sectors. Enormous efforts
have been observed from various publications towards the devel-
opment of supplementary cement-based materials (SCMs) such
as industrial by-products like slag, fly ash, silica fume, etc [2] to
eliminate the use of Portland cement which may reduce the carbon
emissions significantly [3]. In this context, geopolymer technology
has enticed the researchers all across the globe as an alternative to
cement binder. It was originally coined by Glikhovsky in 1957 [4]
but further developed by Davidovits as binder material [5]. It is a

http://dx.doi.org/10.1016/j.conbuildmat.2017.06.066
0950-0618/Ó 2017 Elsevier Ltd. All rights reserved.
818 A. Mehta et al. / Construction and Building Materials 150 (2017) 817–824
technology that involves the production of binders which can be
used in concrete applications produced by polymerization reac-
tions of alumina-silicates with alkaline solutions in the presence
of high temperature [6]. The mechanism involves the polymeric
reactions of silica and alumina, liberated by alkali-activating solu-
tions (mainly hydroxides, and silicates of potassium and sodium)
from the source material, in the presence of high temperature.
Out of various industrial by-products, fly ash can be considered
as most beneficial [7] due to its suitable chemical composition, fine
size and easy availability [8]. Also, the most commonly used alkali-
activating solution is the mixture of hydroxide and silicate of
sodium [9,10]. Geopolymer concrete has been found to have com-
parable or better properties in terms of compressive strength, per-
meability, resistance to aggressive ions and resistance to high
temperature [11,12]. Various parameters that can persuade the
geopolymer concrete properties are the fineness of source material,
sodium silicate to sodium hydroxide ratio in the alkali-activating
solution, sodium hydroxide molarity, different curing methods
and temperatures [13]. Besides these, the inclusion of external
materials such as additional calcium source has also found to affect
its properties significantly [14].
The major advantage of geopolymers over the conventional
concrete is the development of high early age strength as the
geopolymer binders NASH and CASH are the results of polymeric
reaction in the presence of high-temperature curing. Whereas,
the increment in strength values at later ages is not significant,
unlike conventional concrete. Kong and Sanjayan [15] observed
the compressive strength values of geopolymer concrete speci-
mens up to 3 days only which was found comparable to that of
28 days compressive strength of conventional concrete. Other
studies also reported no significant development of compressive
strength after 7 days [9,16]. The aim of this study is to evaluate
the best combination of considered parameters to develop
geopolymer concrete specimens yielding maximum compressive
strength and minimum water absorption. The optimization of mix-
tures is achieved by using Taguchi method considering the param-
eters such as different contents of OPC as fly ash replacement,
different concentrations of sodium hydroxide (NaOH) and different
curing temperatures.
2. Materials and methods
2.1. Materials
Class F Fly ash obtained from Rajiv Gandhi thermal power plant, Northern India
and ordinary Portland cement (OPC) (as an external calcium source) obtained from
the local sources, were used in this study. The physical and chemical properties of
fly ash and OPC were evaluated as shown in Tables 1 and 2. The specific surface area
of fly ash particles was 268 m2/kg and specific gravity was determined as 2.33.
Scanning electron microscopy (SEM) and energy dispersive X-ray spectroscopy
(EDS) analysis were also performed on fly ash and OPC as shown in Figs. 1 and 2,
respectively. Fly ash particles were found to be spherical in shape whereas OPC par-
ticles were found to be more irregular. Also, quartz and mullite were observed as
main phases for fly ash whereas ettringite, portlandite, and calcite were determined
for OPC. Crushed stone aggregates of nominal diameter 12.5 mm were used as
coarse aggregates with specific gravity 2.54 and water absorption 0.98% whereas,
natural river sand obtained from Ghaggar river was used as fine aggregates with
fineness modulus 2.52, specific gravity 2.58 and water absorption 0.25%. The
alkali-activating solution was prepared as the mixture of sodium hydroxide (NaOH)
Table 1
Physical properties of OPC and fly ash.
Physical properties OPC
Standard consistency 33%
Initial setting time 95 min
Final setting time 464 min
Specific gravity 3.12
Fineness (m2/kg) 328
Table 2
Chemical properties of OPC and fly ash.
Oxides OPC (%) Fly ash (%)
Silica Oxide (SiO2) 19.72 38.63
Aluminium oxide (Al2O3) 4.53 15.48
Iron oxide (Fe2O3) 4.59 18.56
Calcium oxide (CaO) 66.23 18.11
Magnesium oxide (MgO) 0.87 2.48
Potassium oxide (K2O) 0.89 0.68
Sodium oxide (Na2O) 0.57 0.89
Sulphur trioxide (SO3) 2.60 5.17
and sodium silicate (Na2SiO3). The NaOH solution was prepared by mixing NaOH
pellets and the distilled water with desired molarity whereas Na2SiO3 solution
was prepared with 16.20% sodium oxide (Na2O), 34.72% silica oxide (SiO2) and
49.08% water. Due to the high temperature of the alkali-activating solution, it
was prepared 24 h prior to its use to bring down its temperature to ambient condi-
tions [17,18].
2.2. Optimum mixture determination
Taguchi method was used to develop the design of experiments and to deter-
mine the optimum parametric combination to yield maximum compressive
strength and minimum water absorption. A robust design of the L16 orthogonal
array was developed for experimentation [19]. Three factors were expected to influ-
ence the strength and absorption characteristics of fly ash based geopolymer con-
crete such as fly ash replacement by OPC, NaOH molarity, and curing
temperature for the constant duration. These parameters with 4 different levels
such as 5, 10, 15 & 20% inclusion of OPC as fly ash replacement; 5, 10, 15 & 20 M
NaOH molarity, and 60, 70, 80 & 90 °C curing temperature were considered as
shown in Table 3. Factors such as aggregates content, admixture dosage (2%) and
curing duration (24 h) were kept as constant. Table 4 shows the different paramet-
ric combination for the design of experiment by Taguchi method. 16 sets of exper-
iments with 3 samples each were studied as L16 for compressive strength as well as
water absorption. After performing various trial mixtures, the final design mixture
was adopted as shown in Table 5.
2.3. Methods
Geopolymer concrete specimens were prepared by mixing fly ash, OPC, coarse
aggregates and fine aggregates together with the alkali-activating solution, which
was prepared 24 h before casting. To maintain the adequate workability, naph-
thalene based admixture was used at 2% by weight of total alkalis (fly ash and
OPC). The materials were mixed inside a pan mixture for about 15 min and the con-
crete was filled in the specimens with proper compaction. For compressive
strength, cube molds of size 150  150  150 mm and for water absorption, the
cylindrical mold of size 100  200 mm were cast. The specimens were kept at room
temperature for about an hour as a rest period and covered by a steel plate to avoid
any loss of moisture. These covered specimens were subjected to oven curing for
24 h. The de-moulded specimens after curing were covered by cling film and kept
at room temperature until its testing age. For compressive strength testing, cubical
concrete specimens were kept inside a compression testing machine (CTM) of
2000 kN capacity at the age of 7 days. The load was applied to the specimens with-
out any jerk until no further load was sustained. For water absorption, discs of size
100  50 mm were cut from the parent cylindrical molds of 100  200 mm and
tested in accordance with ASTM C642 [20] at the age of 7 days. Three specimens
were tested for each mixture and the results were reported as their average.
3. Results and discussions
3.1. Experimental results
Table 6 shows the results of compressive strength and water
absorption for the developed set of experiments. It was observed
that almost all the mixtures had 7 days strength values above
50 MPa which confirmed their potential for the applications where
high early age was required. Maximum strength was observed for
T15 specimens with the average strength value of 64.39 MPa.
These specimens correspond to 20% inclusion of OPC as fly ash
replacement, the 15 M molarity of NaOH and curing temperature
of 70 °C for 24 h. On the other hand minimum water absorption
was obtained as 3.04% for T14 specimens that pertain to 20%
OPC, 10 M molarity and 80 °C curing temperature. Almost similar
results were obtained for T14 and T15 specimens in terms of
 A. Mehta et al. / Construction and Building Materials 150 (2017) 817–824 819

Fig. 1. SEM/EDS analysis of fly ash.

Fig. 2. SEM/EDS analysis of OPC.

Table 3
Factors and levels.

Factors Level 1 Level 2 Level 3 Level 4

A: OPC content (%) 5 10 15 20
B: Molarity of NaOH (M) 5 10 15 20
C: Curing temperature (°C) 60 70 80 90

compressive strength and water absorption. For microstructure
analysis, SEM/EDS and XRD analysis were also performed on T14
specimens as shown in Figs. 3 and 4 respectively. Continuous
and dense microstructure was observed which indicate high
degree of polymerization reactions. In addition to geopolymeric
products like CASH and NASH, coexistence of OPC hydration
product CSH was also observed with the inclusion of OPC in the
system. Similar coexistence was also reported in previous studies
[21–23] as well. Also no cracks were observed in the microstruc-
ture which indicates proper aggregate-binder bonding and
therefore, decreased the voids and water absorption. EDS analysis
showed the presence of silica (Si), alumina (Al) and sodium (Na)
with some amount of oxygen (O), calcium (Ca) and iron (Fe). The
high Si/Al ratio was related to more dissolution in the geopolymer
system making the microstructure more compact. XRD analysis
showed the presence of broad amorphous humps which indicate
the presence of CSH in the geopolymer binder system and
influenced the strength and absorption properties of geopolymer
system [24]. The peaks showed the presence of ettringite, naphe-
line, portlandite and CSH which also confirmed the coexistence
of geopolymer and hydration based products. Napheline was
associated with NASH as polymerization reaction product of
alumina-silica polymer structure whereas portlandite was associ-
ated with the additional hydrated CSH products.
820 A. Mehta et al. / Construction and Building Materials 150 (2017) 817–824

Table 4
Factors and levels in trial mixtures.

Trial Mixture Combination Factors

OPC content (%) Molarity of NaOH (M) Curing temperature (°C)
T1 A1B1C1 5 5 60
T2 A1B2C2 5 10 70
T3 A1B3C3 5 15 80
T4 A1B4C4 5 20 90
T5 A2B1C2 10 5 70
T6 A2B2C1 10 10 60
T7 A2B3C4 10 15 90
T8 A2B4C3 10 20 80
T9 A3B1C3 15 5 80
T10 A3B2C4 15 10 90
T11 A3B3C1 15 15 60
T12 A3B4C2 15 20 70
T13 A4B1C4 20 5 90
T14 A4B2C3 20 10 80
T15 A4B3C2 20 15 70
T16 A4B4C1 20 20 60

Table 5
Design mixture for Taguchi optimization.

Mixture Fly ash OPC Coarse aggregates Fine aggregates Alkali content Molarity of Curing
(kg/m3) (kg/m3) (kg/m3) (kg/m3) (kg/m3) NaOH (M) temperature (°C)
T1 302.1 15.9 1230 662 175 5 60
T2 302.1 15.9 1230 662 175 10 70
T3 302.1 15.9 1230 662 175 15 80
T4 302.1 15.9 1230 662 175 20 90
T5 286.2 31.8 1230 662 175 5 70
T6 286.2 31.8 1230 662 175 10 60
T7 286.2 31.8 1230 662 175 15 90
T8 286.2 31.8 1230 662 175 20 80
T9 270.3 47.7 1230 662 175 5 80
T10 270.3 47.7 1230 662 175 10 90
T11 270.3 47.7 1230 662 175 15 60
T12 270.3 47.7 1230 662 175 20 70
T13 254.4 63.6 1230 662 175 5 90
T14 254.4 63.6 1230 662 175 10 80
T15 254.4 63.6 1230 662 175 15 70
T16 254.4 63.6 1230 662 175 20 60

Table 6
Experimental results for compressive strength and water absorption.

Experiment No Coded value Actual setting Value Compressive strength (MPa) Water absorption (%)
1 2 3 1 2 3
1 1 1 1 5 5 60 48.36 3.97
2 1 2 2 5 10 70 54.79 3.67
3 1 3 3 5 15 80 56.37 3.35
4 1 4 4 5 20 90 55.69 3.47
5 2 1 2 10 5 70 54.31 3.59
6 2 2 1 10 10 60 55.24 3.50
7 2 3 4 10 15 90 59.57 3.24
8 2 4 3 10 20 80 57.94 3.22
9 3 1 3 15 5 80 57.06 3.37
10 3 2 4 15 10 90 60.24 3.17
11 3 3 1 15 15 60 55.76 3.41
12 3 4 2 15 20 70 59.53 3.25
13 4 1 4 20 5 90 57.69 3.24
14 4 2 3 20 10 80 63.67 3.04
15 4 3 2 20 15 70 64.39 3.09
16 4 4 1 20 20 60 56.02 3.38

3.2. Mathematical models
Based on the experiment results obtained in this study, analysis
of variance (ANOVA) for compressive strength and water absorp-
tion was performed as shown in Tables 7 and 8 respectively. It
was carried out at a confidence level of 95%. The purpose of this
analysis was to find out the impact of considered parameters i.e.
OPC inclusion, NaOH molarity and curing temperature, on the
compressive strength and water absorption properties. From the
ANOVA results for compressive strength, it was observed that
 A. Mehta et al. / Construction and Building Materials 150 (2017) 817–824 821

Fig. 3. SEM/EDS analysis of T14 specimen.

65
Experimental
Compressive strength (MPa)

64
Mathematical Model
63
62
61
60
59
58
57
56
T3 T7 T10 T15

Fig. 5. Confirmation of experimental results with developed model for compressive

strength.

Fig. 4. XRD analysis of T14 specimen.

Table 7
ANOVA for compressive strength.

Source of Variation Sum of Squares Degrees of Freedom Mean Square F-value Contribution (%)
A: OPC content (%) 92.447 3 30.816 21.54 42.58
B: Molarity of NaOH (M) 52.175 3 17.392 12.16 24.49
C: Curing Temperature (°C) 63.901 3 21.300 14.89 29.43
Error 8.583 6 1.430 – 3.5
Total 217.106 15 – – 100

Table 8
ANOVA for water absorption.

Source of Variation Sum of Squares Degrees of Freedom Mean Square F-value Contribution (%)
A: OPC content (%) 0.3940 3 0.1313 52.89 47.74
B: Molarity of NaOH (M) 0.1658 3 0.0553 22.26 20.09
C: Curing Temperature (°C) 0.2505 3 0.0835 33.62 30.35
Error 0.0149 6 0.0025 – 1.82
Total 0.8253 15 – – 100
822 A. Mehta et al. / Construction and Building Materials 150 (2017) 817–824

6 ture (denoted by T) individually as well as their two-factor interac-

Experimental tion, R & M, M & T and R & T.
5.5
Mathematical Model
Water Absorption (%)

5 CS ¼ 18:7166 þ 0:5399R þ 0:2114M þ 1:7143T  0:0067R2

4.5  0:0586M 2  0:0122T 2 þ 0:0045RM þ 0:0187RT
4 þ 0:0022MT ð1Þ
3.5 2
R = 0.98
3 and

2.5
2
T3 T8 T10 T14
Fig. 6. Confirmation of experimental results with developed model for water
absorption.
OPC inclusion as fly ash replacement was the most significant
parameter with the highest contribution of 42.58% whereas other
parameters such as molarity of NaOH and curing temperature
had the contribution of 24.49% and 29.43% respectively. Similarly,
from the ANOVA results of water absorption, OPC inclusion again
showed the highest contribution of 47.74% in comparison to other
considered parameters such as NaOH molarity and curing temper-
ature, which contributed 20.09% and 30.35% respectively. For both
the properties, the main governing factor was the inclusion of OPC
as fly ash replacement in comparison to other two parameters. OPC
inclusion was directly related to the additional calcium in the mix-
ture which had the tendency to quickly react with the alkalis in the
system and resulted in additional hydration products with extra
heat. This additional heat also enhanced the effective curing tem-
perature of the geopolymer system [25] and improved the com-
pressive strength and water absorption significantly [26].
Based on experimental results mathematical models for com-
pressive strength (CS) and water absorption (WA) was developed
using polynomial regression equation. The model consists of all
the parameters i.e. OPC inclusion as fly ash replacement (denoted
by R), the molarity of NaOH (denoted by M) and curing tempera-
WA ¼ 7:3345  0:0513R  0:0706M  0:0744T þ 0:0011R2
þ 0:0026M 2 þ 0:0005T 2 þ 0:0009RM  0:0003R
 0:0002MT ð2Þ
R2 = 0.97
Where,
CS = compressive strength
WA = water absorption
R = fly ash replacement by OPC (%)
M = molarity of NaOH (M)
T = curing temperature (°C)
A high value of the coefficient of determination (R2) was
obtained for both compressive strength and water absorption
models as 0.98 and 0.97 respectively which indicate a good corre-
lation between the experimental and model results. For their con-
firmation, the experimental values of compressive strength and
water absorption were compared to their model output values.
As OPC inclusion (as fly ash replacement) was found to be the most
significant factor, for each level of OPC inclusion (5, 10, 15 & 20%)
mixtures with maximum strength values as well as minimum
water absorption were chosen. For example, for compressive
strength, mixtures T3, T7, T10 & T15 and for water absorption, mix-
tures T3, T8, T10 & T14 were chosen for the comparison as shown
in Figs. 5 and 6 respectively. It was observed that the developed
mathematical models, for determining the performance of
geopolymer concrete in terms of compressive strength and water
absorption, agree well with the experimental test results.

Fig. 7. SN ratio curves for compressive strength.

 A. Mehta et al. / Construction and Building Materials 150 (2017) 817–824
Fig. 8. SN ratio curves for water absorption.
3.3. Signal-to-Noise ratio (SNR)
Signal to noise ratio (SNR) was used to determine the optimum
parametric combination for the considered factors. In general, SNR
characteristics may be divided into following categories:
S y
¼ 10 log 2
N s
1 X  pressive strength and water absorption were considered. The mix-
S
¼ 10 log y2
N n
 
S 1 X1
¼  log
N n y2
For Eq. (3), the nominal value can be considered as the best
characteristic whereas, for Eqs. (3) and (4), smaller and larger val-
ues can be considered as optimum respectively. In this study, Eq.
(5) was used for compressive strength whereas Eq. (4) was used
for compressive strength in determining their best characteristic
combination as shown in Figs. 7 and 8 respectively. It was observed
that compressive strength increased with the increase in OPC
inclusion with the maximum at 20%. Also, it increased with the
increase in molarity of NaOH up to 15 M and curing temperature
up to 80 °C, beyond these values, decrease in compressive strength
was observed. Similar trend was also observed for water absorp-
tion where minimum value was achieved up to 20% OPC, 15 M
NaOH molarity and 80 °C temperature curing and beyond these,
it increased. It was attributed to the fact that with the increase
in calcium content in the form of OPC, additional hydration prod-
ucts were induced along with geopolymeric binders which
improved the microstructure and lowered the voids as well. On
the other hand, the increase in NaOH molarity was directly related
to more liberation of silica and alumina from the source material
and hence increased the geopolymer binder products. Also, as
geopolymer mechanism involves the polymerization reactions
which accelerate the formation of hard structure at higher temper-
atures [26], with the increase in temperature, microstructure
becomes more tough and compact. From SNR, the optimum mix-
823
ture for the maximum compressive strength and minimum water
absorption was observed to be A4B3C3 (20% OPC, 15 M molarity
and curing temperature 80 °C).
4. Conclusions
ð3Þ
Three parameters which were expected to influence the com-
ð4Þ tures were designed using Taguchi analysis and the experimental
results were used to develop mathematical models. Following con-
clusions were drawn:
ð5Þ
1. Fly ash based geopolymer concrete with high 7 days compres-
sive strength of 64.39 MPa was obtained for the mixture with
20% Ordinary Portland cement (OPC) (as fly ash replacement),
sodium hydroxide molarity of 15 M and at a curing temperature
of 70 °C for 24 h. Similarly 7 days water absorption of 3.04% was
observed for specimen with 20% OPC, 10 M sodium hydroxide
and curing temperature of 80 °C for 24 h.
2. The microstructure of T15 specimen with maximum compres-
sive strength found to be dense and compact with no voids.
Calcium-silicate hydrate was found to coexist with Calcium-
alumino-silicate hydrate and sodium-alumino-silicate hydrates
which improved strength as well as absorption characteristics.
3. From Analysis of Variance, the inclusion of additional calcium
(in the form of OPC as fly ash replacement) was found to be
the most significant factor in controlling the compressive
strength as well as water absorption.
4. The mathematical models were proposed with a high degree of
determination which can be utilized for the evaluation of com-
pressive strength and water absorption with the considered
parameters.
5. From Signal-to-Noise ratio, the optimal parametric combination
for maximum compressive strength and minimum water
absorption was obtained at parametric combination A4B3C3
(fly ash replacement by OPC at 20%, 15 M sodium hydroxide
and curing temperature 80 °C for 24 h).
824 A. Mehta et al. / Construction and Building Materials 150 (2017) 817–824

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