Arab J Sci Eng (2016) 41:12631271

DOI 10.1007/s13369-015-1906-4

RESEARCH ARTICLE - CIVIL ENGINEERING

Compressive strength, Bending and Fracture Characteristics of

High Calcium Fly Ash Geopolymer Mortar Containing Portland
Cement Cured at Ambient Temperature
Tanakorn Phoo-ngernkham1 Vanchai Sata2 Sakonwan Hanjitsuwan3
Charoenchai Ridtirud4 Shigemitsu Hatanaka5 Prinya Chindaprasirt2

Received: 24 April 2015 / Accepted: 6 October 2015 / Published online: 23 October 2015
King Fahd University of Petroleum & Minerals 2015

Abstract This article presented the compressive strength,
modulus of rupture and fracture characteristics of high cal-
cium fly ash (FA) geopolymer mortars containing Portland
cement type I (PC) with different sodium hydroxide (NaOH)
concentrations (6, 10 and 14 molars). PC was added at the
dosages of 0, 5, 10 and 15 % by weight of solid powder binder.
Sodium silicate (Na2 SiO3 ) and NaOH solutions were used as
the alkali activators. Na2 SiO3 to NaOH ratio of 2.0, alkaline
liquid to binder ratio of 0.60, sand to binder ratio of 1.00 and
curing at ambient temperature were used for all mixtures.
Test results indicated that the use of PC as additive enhanced
compressive strength, modulus of rupture and fracture char-
acteristics of high calcium fly ash geopolymer mortar and
NaOH concentrations also had significant affect on these
properties. The use of 10 % PC with 14M NaOH resulted
B Prinya Chindaprasirt
prinya@kku.ac.th
1
Research Center for Advances in Civil Engineering and
Construction Materials, Program in Civil Engineering,
Faculty of Engineering and Architecture, Rajamangala
University of Technology Isan, Nakhon Ratchasima, 30000,
Thailand
2 Sustainable Infrastructure Research and Development Center
(SIRDC), Department of Civil Engineering, Faculty of
Engineering, Khon Kaen University, Khon Kaen, 40002,
Thailand
3
Program of Civil Technology, Faculty of Industrial
Technology, Lampang Rajabhat University, Lampang, 52100,
Thailand
4 Department of Civil Engineering, Faculty of Engineering,
Rajamangala University of Technology Isan, Khon Kaen
campus, Khon Kaen, 40000, Thailand
5 Department of Architecture, Faculty of Engineering, Mie
University, Mie, 514-8504, Japan
in high calcium FA geopolymer mortar with improved mod-
ulus of rupture and fracture characteristics.
Keywords Geopolymer High calcium fly ash Portland
cement NaOH concentration Fracture characteristics
Ambient temperature
1 Introduction
Manufacturing of Portland cement is an energy intensive
process and releases a large amount of greenhouse gas [1].
The use of pozzolan to replace part of Portland cement is,
therefore, quite attractive. One of the novel methods to reduce
the use of Portland cement in concrete industry is the use of
alternative binder such as geopolymer [2,3]. Geopolymer is
normally made from silica and alumina-rich source materials
such as fly ash, bottom ash, granulated blast furnace slag and
calcined kaolin activated with high alkali solutions [35].
In Thailand, the annual output of lignite fly ash from Mae
Moh power station is around 3.0 million tons [6]. Chin-
daprasirt et al. [7] reported that around 1.8 million tons of
this fly ash is used as pozzolanic material in the cement and
concrete industry; however, a large portion of this fly ash
is still left over and discarded at landfill site which poses a
serious environmental problem. This fly ash has been shown
to be a suitable source material for making geopolymer [8
10]. In addition, the mechanical properties, fire resistance,
acid resistance of geopolymer binder are superior to those of
Portland cement [1113].
Normally, the alkali solution is used for the activation by
dissolving of Si4+ and Al3+ ions from the source material
and from geopolymeric material. The most commonly used
alkaline activators are sodium hydroxide and sodium silicate
solutions [3]. Somna et al. [8] reported that sodium hydrox-

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Table 1 Chemical
Materials SiO2 Al2 O3
compositions of FA and PC (by
weight) FA 29.32 12.96
PC 20.80 4.70
ide concentration significantly affects both the compressive
strength and structure of geopolymers. Sodium hydroxide
concentration in the aqueous phase of geopolymeric system
affects the dissolution process as well as the bonding of solid
particles in the final structure [12,14]. Rattanasak and Chin-
daprasirt [15] reported that the leaching of Si4+ and Al3+
ions depends on sodium hydroxide concentration and leach-
ing time which affects the geopolymerization and mechanical
properties of hardened geopolymer.
At ambient temperature of 25 C, the strength develop-
ment of high calcium fly ash geopolymer is quite low [16]
even though this FA consists of a substantial CaO content.
In order to improve the strength development of high calcium
fly ash geopolymer, improvements in strength development
of fly ash geopolymers have thus been studied by several
researchers [1719]. The incorporation of Portland cement
in the high calcium fly ash geopolymer is beneficial as the
heat generated from the exothermic reaction of Portland
cement hydration can assist the geopolymerization process
[16,2022]. Furthermore, the existence of calcium produces
calcium silicate hydrate (CSH) gel which co-exists with
geopolymer gel and results in higher compressive strength
geopolymer [19].
One of the important properties of cementitious materials
is its fracture characteristics which are related to the for-
mation and propagation of cracks in the materials [23]. It
depends on the mechanical interaction between aggregate
and binder matrix [24]. Therefore, it is desirable to evaluate
the fracture properties of cement and concrete materials for
the proper design and safety of structure [25]. This property
is related to the mechanical behaviors of materials under the
loading and failure conditions.
Therefore, this research aims to study on the compressive
strength, modulus of rupture and fracture characteristics of
high calcium fly ash geopolymer mortars containing Port-
land cement with various sodium hydroxide solutions. The
obtained results should be very beneficial to the understand-
ing and to the future applications of geopolymer mortars as
alternative repair material.
2 Experimental Details and Testing Analysis
2.1 Materials
The binder materials used in this study were high calcium fly
ash (FA) from Mae Moh power plant in northern Thailand
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Arab J Sci Eng (2016) 41:12631271
Fe2 O3 CaO MgO K2 O Na2 O SO3 LOI
15.64 25.79 2.94 2.93 2.83 7.29 0.30
3.40 65.30 1.50 0.40 0.10 2.70 0.90
and Portland cement Type I (PC). The liquid portions in the
mixture were sodium hydroxide (NaOH) of 6, 10 and 14 M
concentrations and sodium silicate (Na2 SiO3 ) with 13.89 %
Na2 O, 32.15 % SiO2 and 46.04 % H2 O by weight. Local river
sand with specific gravity of 2.63 and fineness modulus of
1.80 were used.
The chemical composition of FA and PC is shown in
Table 1. The specific gravities of FA and PC were 2.61 and
3.16, respectively. The median particle sizes of FA and PC
were 8.5 and 14.6 m with the corresponding Blaine fine-
nesses of 4300 and 3600 cm2 /g, respectively.
2.2 Mix Proportion of Geopolymer Mortars
The mix proportions of geopolymer mortars (GPM) are
shown in Table 2. Constant liquid alkaline to binder ratio
of 0.60, Na2 SiO3 to NaOH ratio of 2.0 and sand to binder
ratio of 1.0 were used. The effects of NaOH concentrations
(6, 10 and 14 M) were also studied. Four levels of PC replace-
ment by FA of 0, 5, 10 and 15 % by weight were used. For the
mixing of mortars, NaOH and Na2 SiO3 solutions were firstly
mixed together and used as the liquid solution. The FA, PC
and sand were dry mixed until the mixture was homogenous.
Right after, the liquid solution was added and the mixing
of mortars was done for 5 min. In this paper, the geopoly-
mer mortars are specified by the NaOH molar and Portland
cement content. For example, 6M10PC stands for geopoly-
mer mixture with 6 M NaOH and 10 % PC replacement.
3 Testing and Analysis
3.1 Compressive Strength of Geopolymer Mortars
Fresh mortar was cast in 505050 mm3 cube molds for the
compressive strength test in accordance with ASTM C109
[26]. The samples were demolded at the age of 1 day and
immediately wrapped with vinyl sheet to protect moisture
loss and kept in the 25 C controlled room. The compressive
strengths were tested at the ages of 28 days and the reported
results were the average of three samples.
3.2 Modulus of Rupture of Geopolymer Mortars
The fresh mortar was cast in 75 75 75 mm3 prisms molds
for the modulus of rupture (MOR) tests in accordance with
Arab J Sci Eng (2016) 41:12631271 1265

Table 2 Mix proportions of

Mix no. Mix symbol FA (g) PC (g) Sand (g) NaOH (g) Na2 SiO3 (g)
geopolymer mortars
6M 10 M 14 M

1 6M0PC 100 100 20 40

2 6M5PC 95 5 100 20 40
3 6M10PC 90 10 100 20 40
4 6M15PC 85 15 100 20 40
5 10M0PC 100 100 20 40
6 10M5PC 95 5 100 20 40
7 10M10PC 90 10 100 20 40
8 10M15PC 85 15 100 20 40
9 14M0PC 100 100 20 40
10 14M5PC 95 5 100 20 40
11 14M10PC 90 10 100 20 40
12 14M15PC 85 15 100 20 40

the ASTM C293-02 [27]. The samples were demolded and Alig is the area of the ligament that was intact before the test
cured the same way as the compressive strength samples. (m2 ).
At the age of 28 days, the samples were tested in deflection For the determination of fracture toughness, the term frac-
control with loading rate of 0.05 mm/min [25]. The reported ture toughness or critical stress intensity factor (KIC ) was
results were the average of three samples. used to indicate the magnitude of stress concentration that
exists in front of the crack tip when the crack starts to prop-
3.3 Fracture Characteristics of Geopolymer Mortars agate [24]. The most common method of calculation of the
critical stress intensity factor is to use the peak load from
The fresh mortar samples were cast in 7575300 mm3 long three-point bending test of notched beam [24,25,29]. The
beams for fracture characteristics test. They were demolded fracture toughness or critical stress intensity factor (KIC ) was
at the age of 1 day and immediately wrapped with vinyl calculated using Eqs. (2)(4) [28].
sheet to protect moisture loss and kept in the 25 C controlled
room. After curing, the samples were cut with a notch height 3Pl 
KIC = (a0 )F (a) (2)
to beam depth (a0 /d) ratio of 0.4 and notch width to notch 2bd 2
height (w0 /a0 ) ratio of 0.2 in the middle of the beam as
shown in Fig. 1. The fracture characteristics were tested at where F (a) is
the age of 28 days using three-point bending. The tests were
     2 
performed in deflection control mode with constant loading 1/ 1.99 ad0 (1 ad0 2.153.93 ad0 +2.7 ad0
rate of 0.05 mm/min [25], and the deflection data at middle   1.5 
span were recorded by LVDT. The reported results were the 1+2 ad0 1 ad0
average of three samples. (3)
The fracture energy (GF ) is the energy needed to cre-
ate a crack of unit area and can be calculated by measuring Therefore, this could be re-written as
the area under load-defection curve of geopolymer mortar
notched beam and deformation at the mid-span of concrete  a   a 2
3Pl 0 0
beam. The fracture energy or specific fracture energy (GF ) KIC = a0 1.93 3.07 + 14.53
2bd 2 d d
was calculated from the work of fracture using Eq. (1) [28].
 a 3  a 4

0 0
25.11 + 25.80 (4)
W0 + mgmax d d
GF = (1)
Alig
where K I C is fracture toughness or critical stress intensity
where G F is fracture energy (N/m), W0 is the area under factor (MPa-mm0.5 ), P is the maximum load (N), l is the
the load deflection curve (N-m), m is the mass of the beam span length of beam (mm), b is the width of beam (mm),
between supports (kg), g is the acceleration due to gravity d is the depth of beam (mm), and a0 is the depth of notch
(m/s2 ), max is the deflection at final failure of beam (m), and (mm).

123
1266
Fig. 1 Samples for fracture test
4 Results and Discussions
4.1 Compressive Strength of Geopolymer Mortars
The results of compressive strength of geopolymer mortar
are shown in Fig. 2. The increase in both PC replacement
level and NaOH concentration resulted in the increase in
compressive strengths of mortars. For example, the compres-
sive strengths of 6M0PC, 6M10PC, 14M0PC and 14M10PC
mortars were 38.5, 45.3, 56.0 and 63.3 MPa, respectively.
Also, the increase in PC replacement resulted in a reduction
in setting time of geopolymer mortars as shown in Fig. 3.
The increase in calcium content significantly accelerated the
setting and hardening of geopolymer system [16]. Lee and
van Deventer [30] reported that additional calcium content
increased its solidification rate and cause rapid hardening;
therefore, the improvement in strength of mortar was due
to the increase in the reaction products with additional C
SH and CASH gel co-existed with N-A-S-H gel [18].
With regard to the effect of NaOH concentration, the strength
and setting time of geopolymer mortar increased with the
increase in NaOH concentration. As shown in Fig. 3, the
high NaOH concentrations resulted in the delay of setting
Fig. 2 Compressive strength of geopolymer mortars
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Arab J Sci Eng (2016) 41:12631271
Fig. 3 Setting time of GPM
time of geopolymer mortars. This was due to the increase in
dissolution of silica and alumina, whereas the leaching out of
calcium from raw materials was hindered [6]. The increase
in the leaching out of Si4+ and Al3+ ions from FA particles at
high NaOH concentration also contributed to an increasing
of its strength due to subsequent formation of N-A-S-H gel
and thus improved the geopolymerization [15].
The SEM of fracture surfaces of high calcium FA geopoly-
mer pastes with various PC replacements cured at ambient
temperature for 28 days are given in Fig. 4. The results of
compressive strength with various PC replacements agreed
well with the SEM analyses.
The SEM of geopolymer pastes without PC replacement
showed loose matrices with large number of non-reacted
and/or partially reacted FA particles embedded in poor matri-
ces. Normally, the geopolymerization of high calcium FA
was slow at ambient temperature and needed temperature
curing to accelerate the strength development [16]. With
increasing level of PC replacement, the dense structure with
continuous matrix and less number of FA particles were
observed as illustrated in Fig. 4b, d. Pangdaeng et al. [16]
claimed that the increasing calcium content enhanced the
degree of reaction from an exothermal reaction with liberated
Arab J Sci Eng (2016) 41:12631271 1267

Fig. 4 SEM of geopolymer

pastes. a 10M0PC, b 10M5PC,
c 10M10PC, d 10M15PC

heat which resulted in additional CSH and/or CAS

H from the reaction of PC and leached calcium from FA
co-existing with NASH gel. Therefore, this resulted in
overall to strength development of high calcium FA geopoly-
mer containing PC.

4.2 Modulus of Rupture of Geopolymer Mortars

The MOR of geopolymer mortars as shown in Fig. 5

increased as increasing in both replacement level of PC and
NaOH concentration up to the threshold level. The results fol-
lowed similar trend to that of the compressive strength results.
The increase in MOR with the increase in replacement level
of PC from 0 to 10 % was due primarily to the formation of C
SH and CASH which coexisted with the N-A-S-H gel.
However, the incorporation of high amount of PC (15 %) and
high NaOH concentration (14 M) resulted in a slight decline
in the MOR of mortar. For instance, the MORs of 14M0PC,
14M5PC, 14M10PC and 14M15PC mortars were 7.07, 8.51,
8.96 and 7.49 MPa, respectively. At high NaOH concentra-
tion, polycondensation was hindered and the excess OH ion
concentration caused early aluminosilicate gel precipitation
[33]. This affected the beneficial effect of PC incorporation
especially at the high replacement level (15 %) and thus low-
ered the strengths of geopolymer mortars.
The graph between compressive strength and MOR of
geopolymer mortars is shown in Fig. 6. MOR increased lin-
early with increasing square root of compressive strength and
Fig. 5 Modulus of rupture of geopolymer mortars
the finding conformed with those reported by Pacheco-Torgal
et al. [31] and Sofi et al. [32]. The equations used for calcula-
tions are normally used for concrete. For mortar specimens,
the aggregate size is smaller and thus the interpretation and
further use of results should be done with care. The relation-
ship between modulus of rupture and compressive strength
can be written as

M O R = 2.78 f c 13.95 (5)
where M O R is the modulus of rupture (MPa) and f c is the
compressive strength (MPa).

123
1268
Fig. 6 Relationship between compressive strength and modulus of
rupture of geopolymer mortars compared with previously published
results of geopolymer mortar and Portland cement mortar
It can be observed from Fig. 6 that the MOR of mor-
tars expressed as a function of compressive strength was
higher than those of Portland cement concrete (PCC) pre-
dicted by ACI 318 [33]. The MORs of mortars in this
study are of the same order as those of geopolymer mortars
(GPM) and Portland cement mortars (PCM) given by Sofi
(a)
(c)
Fig. 7 Load-deflection of geopolymer mortars. a 6M NaOH, b 10M NaOH, c 14M NaOH, d Comparison between NaOH concentration
123
Arab J Sci Eng (2016) 41:12631271
et al. [32] and Qiao et al. [34], but were slightly lower than
those of geopolymer mortars made from mine waste mud,
calcium hydroxide and 24M NaOH reported by Pacheco-
Torgal et al. [31] and Pacheco-Torgal et al. [35]. This was
due to the differences in the source materials and NaOH
concentrations.
4.3 Fracture Energy Of Geopolymer Mortars
The load-defection curves of geopolymer mortar notched
beam are shown in Fig. 7. The results of load-defection
curve showed that the applied load increased with increase
in replacement level of PC and NaOH concentration similar
to the behaviors of MOR of mortar. According to Fig. 8, the
fracture energy of mortars increased with NaOH concentra-
tion which was due to the increase in geopolymer products.
However, there was an indication that the rate of fracture
energy tended to decrease with very high NaOH concentra-
tion. This was similar to the results of strength of geopolymer
at high NaOH concentration. The fracture energy values of
geopolymer mortar in this study agreed with that of Sarker et
al. [24] who reported that the fracture energy increased with
compressive strength.
(b)
(d)
Arab J Sci Eng (2016) 41:12631271 1269

Fig. 8 Fracture energy of geopolymer mortars Fig. 9 Fracture toughness of geopolymer mortars

4.4 Fracture Toughness of Geopolymer Mortars

The results of fracture toughness or critical stress intensity

factor (KIC ) of geopolymer mortars are shown in Fig. 9. The
value of fracture toughness indicated the stress concentration
in front of the crack tip when the crack starts to propagate. The
fracture toughness of mortars slightly increased with increas-
ing in NaOH concentrations and the addition of a proper
amount of PC. The results corresponded well with those of
compressive strength and MOR behaviors. A slight decrease
in fracture toughness was also observed from incorporation
of high amount of 15 % PC for mix with high NaOH concen-
trations similar to the case of MOR. This was because the
excess OH ion concentration caused early aluminosilicate
gel precipitation [30] and polycondensation was hindered at Fig. 10 Relationship between fracture toughness and compressive
strength of geopolymer mortars compared with previously published
high NaOH concentration [36]. results of geopolymer concrete, Portland cement mortar and Portland
The relationship between fracture toughness and compres- cement concrete
sive strength of geopolymer mortar is shown in Fig. 10. The
fracture toughness linearly increases with the square root of
ultimate compressive strength. Again, it should be pointed parison are the values of fracture toughness of geopolymer
out here that the equations used for calculations are used for concrete (GPC) and Portland cement concrete (PCC) which
concrete. The relationship between fracture toughness and were higher than those of the geopolymer mortar as expected.
compressive strength of gepolymer mortar from this work
can be written as

5 Conclusions
K I C = 4.30 f c 18.37 (6)
Based on the results of this study, the following conclusions
where K I C is the fracture toughness (MPa-mm0.5 ) and f c
is could be drawn.
the compressive strength (MPa).
As shown in Fig. 10, the fracture toughness values of mor- (1) The use of high NaOH concentration and the addition
tar in this study followed the same trend with those of Sarker of a proper amount of PC enhanced the compressive
et al. [24] and Bharatkumar et al. [25] which indicated that strength, modulus of rupture and fracture characteris-
the fracture toughness tended to increase with the compres- tics of the high calcium fly ash geopolymer mortars.
sive strength. The values of fracture toughness of mortars These properties increased with increase in NaOH con-
are similar to that of Portland cement mortar (PCM) given tent from 6 to 14 M due to the increase in the leaching
by Mindess and Nadeau [37]. Also given in Fig. 10 for com- out of Si4+ and Al3+ ions from the FA particles at high

123
1270
NaOH concentration and the subsequent formation of
NASH gel.
(2) The compressive strength, modulus of rupture, frac-
ture energy and fracture toughness of the mortars also
increased with the replacement level of PC from 0 to
10 % due primarily to the increase in the reaction prod-
ucts within geopolymer matrix.
(3) The incorporation of high amount of PC (15 %) with
high NaOH concentration (14 M) resulted in a slight
decline in these properties of high calcium geopolymer
mortars, because the excess of hydroxide ion concentra-
tion caused early aluminosilicate gel precipitation which
affected the beneficial effect of PC incorporation.
(4) The geopolymer mortar with 14M NaOH and 10 %
PC showed best results with 28-day compressive
strength, modulus of rupture, fracture energy and frac-
ture toughness of 63.3, 8.96 MPa, 54.81 N/m and 18.21
MPa-mm0.5 , respectively.
Acknowledgments This work was supported by the Higher Educa-
tion Research Promotion and National Research University Project of
Thailand, Office of the Higher Education Commission, through the
Advanced Functional Materials Cluster of Khon Kaen University, and
the Thailand Research Fund (TRF) and Khon Kaen University under
the TRF Senior Research Scholar, Grant No. RTA5780004.
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