Composites: Part B 58 (2014) 371–377

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Composites: Part B
journal homepage: www.elsevier.com/locate/compositesb

The influence of the NaOH solution on the properties of the fly ash-based

geopolymer mortar cured at different temperatures
Gökhan Görhan ⇑, Gökhan Kürklü
Afyon Kocatepe University, Faculty of Engineering, Department of Civil Engineering, Afyonkarahisar, Turkey

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

Article history: In this study, geopolymer mortar was produced using Class F fly ash from the thermal power plant in
Received 6 June 2013 Kütahya Seyitömer (Turkey). The changes caused by the geopolymerization on the properties of the final
Received in revised form 27 September 2013 product were investigated by applying curing on geopolymer mortars in different NaOH concentrations
Accepted 27 October 2013
at different temperatures and for different curing times. The purpose of this process was to determine the
Available online 9 November 2013
relationship between alkali solution concentration, curing temperature and curing time. In order to
determine the effect of NaOH concentration on geopolymer mortars, three different molarities of NaOH
Keywords:
concentrations (3 M, 6 M and 9 M) were used together with sodium silicate (water glass) solution. The
B. Physical properties
B. Porosity
samples were cured at two different temperatures (65 and 85 °C). Physical properties such as porosity,
D. Mechanical testing bulk density, apparent density and water absorption, and mechanical properties such as flexural strength
E. Cure and compressive strength were determined from the 7-day geopolymer mortar samples after the curing
Geopolymer process. As a result, this study determined that curing temperature and curing time had an effect on the
physical properties of the geopolymer mortars. It was observed that NaOH concentration had a clear
effect on the properties of the mortar cured at 85 °C. Compressive strength values of 21.3 MPa and
22 MPa were obtained from the mortar of 6 M concentration cured at 65 °C for 24 h and from a sample
of the same mortar cured at 85 °C, respectively. Compressive strength values of the geopolymer mortars
cured at 85 °C increased depending on the curing time and the increase in NaOH concentration. Given the
strength values obtained, the optimal thermal curing temperature and the optimal NaOH concentration
were 85 °C and 6 M, respectively.
Ó 2013 Elsevier Ltd. All rights reserved.

1. Introduction The concentration of the activator has a significant effect on the

A new form of materials with cement characteristics called geo-
polymer has been developed in recent years [1]. Alkaline activa-
tion, usually referred to as geopolymerization, is defined as a
chemical process which alters the glassy constituents in well-com-
pacted and cement-featured composites. A strong alkaline medium
is necessary to increase the surface hydrolysis of the particles of
raw materials with a dissolution consisting of a certain amount
of silica and alumina found in materials during polymerization.
This medium can be obtained by single or combined alkaline solu-
tions referred to as activators [2].
Alkali activator solutions play an important role in the dissolu-
tion of Si and Al oxides. Hence, geopolymers are synthesized by
mixing the most common alkaline activators that are strong alka-
line solutions such as sodium hydroxide (NaOH), potassium
hydroxide (KOH), potassium silicate or sodium silicate with alumi-
nosilicate reactive materials [3–10].
⇑ Corresponding author. Tel.: +90 272 2281423; fax: +90 272 2281422.
E-mail addresses: ggorhan@aku.edu.tr (G. Görhan), kurklu@aku.edu.tr (G.
Kürklü).
compressive strengths of the geopolymers. The ideal concentration
of the activator increases the strength of the geopolymer. Apart
from the ideal concentration, some losses may occur in the
mechanical properties of the material due to the free OH ions in
the alkali-activated matrix which can change the geopolymer
structure of the material. Age and curing temperature of the geo-
polymers are other variables which have an effect on the compres-
sive strength of the samples. However, for these variables to be
effective, sufficient concentration of activator must be present in
the medium during geopolymerization because NaOH concentra-
tion has a greater effect on the strength values than on the curing
temperature and curing time values [2,11,12].
Geopolymers are generally formed by fly ash activated at low
temperatures. Fly ash is an industrial waste with pozzolanic prop-
erties obtained from thermal power plants and used instead of ce-
ment in concrete construction. SiO2 and Al2O3 in the fly ash react
with calcium hydroxide formed as a result of hydration of Portland
cement and start a pozzolanic reaction. For this reason, fly ash can
be used instead of Portland cement [1].
Fly ash contains high levels of amorphous silica and alumina
and is often mixed with alkaline solution to dissolve them. Silicates

1359-8368/$ - see front matter Ó 2013 Elsevier Ltd. All rights reserved.
http://dx.doi.org/10.1016/j.compositesb.2013.10.082
372 G. Görhan, G. Kürklü / Composites: Part B 58 (2014) 371–377
start to dissolve when the fly ash come into contact with alkali
solution. Fly ash can be used as a source material in the production
of geopolymers because geopolymerization is essentially based on
the alumina-silicate chain. However, the type and concentration of
the alkali solution play an important role in the solution of the fly
ash. The solubility of Al3+ and Si4+ ions in sodium hydroxide solu-
bility is higher than in potassium hydroxide solution [13,14].
Therefore, NaOH has an important effect on the structure and the
compressive strength of the geopolymers [15]. Si, Al and other
minor ions begin to dissolve when the fly ash come into contact
with NaOH. The amount of dissolution depends on the NaOH
concentration and dissolution time [1]. The NaOH concentration
affects the dissolution process as well as the binding of solid parti-
cles in the geopolymeric system’s final structure of the aqueous
phase [15]. The mixture of fly ash with 10 molarity (M) of NaOH
is suitable for the geopolymer synthesis [1].
The prepared mixture can be subjected to curing at room tem-
perature or at a given temperature. Aluminosilicate reactive mate-
rials dissolve in strong alkaline solutions and free SiO4 and AlO4
tetrahedral structure forms. However, the reaction of the fly ash
in the production of geopolymers is low at ambient temperatures
[3]. Therefore, the geopolymerization process through which the
material can achieve high compressive strength at given tempera-
tures between 40 and 95 °C can develop [7,12,15,16]. The micro-
structure of the fly ash geopolymers contains aluminosilicate gel,
unreacted fly ash and other crystal phases [17].
Previous studies have concluded that Class F fly ash is a good
source for geopolymers [18] and that NaOH is better than other
activators for the activation of the fly ash in the production of geo-
polymers. When NaOH is used together with water glass, the com-
pressive strength of the geopolymer material is higher than when
only NaOH is used. The reason behind this is the fact that in the
geopolymerization process, water glass increases the reaction
products in which the Si content is higher, and provides more
mechanical strength [19]. Other studies show that when using
the water glass with alkaline activators, compressive and flexural
strength increase [4]; however when water glass is used together
with NaOH, instead of using only NaOH, samples gain significant
strength even in one day [20,21]. However, water glass in powder
form exhibits lower performance than water glass in liquid form
[4].
Some studies in the literature have tested combinations of dif-
ferent curing times and temperatures with NaOH concentrations.
Among these studies, researchers found both geopolymers in
which fly ash and bottom ash were used [22], as well as geopoly-
mers which were synthesized with fly ash, kaolin, sodium silicate
solution and NaOH [7]. In addition, other studies in the literature
are produced light inorganic polymers by synthesizing Class F fly
ash, metakaolin and lightweight aggregates with NaOH sodium sil-
icate solution [23] or produced polymers by using fly ash and so-
dium silicate solution [24], preparation and characterization of
new geopolymer-epoxy resin hybrid mortars [25] and some other
studies synthesized 7-day fly ash-based geopolymers [26] and pro-
duced 7-day fly ash-based geopolymer mortars [27]. The previous
studies generally focused on geopolymer paste. In these studies,
geopolymer materials were subjected to long curing times, and
long periods of time were taken into account for the detection of
their properties. However, in the current study, NaOH and sodium
silicate solution (water glass) were used to activate the Class F fly
ash in order to determine the physical and mechanical properties
of the synthesized geopolymer materials in a short period of time.
The changes in the geopolymerization process and the properties
of the final product were investigated by curing geopolymer mor-
tars, which were prepared using alkali-activated fly ash and
crushed sand, with differing NaOH concentrations, temperatures,
and lengths of time. Thus, the changes in the properties of the
geopolymer mortars in short periods of time were revealed by
detecting the relationships between the alkali solution concentra-
tion, curing temperature and curing time.
2. Materials and methods
2.1. The characterization of the fly ash
In this study, fly ash materials obtained from the Seyitömer
Power Station, in Kütahya, Turkey were used. Chemical analysis
of fly ash was carried out with XRF (Rigaku ZSX Primus). The min-
eralogical analysis was carried out on powdered samples by XRD
0
(Shimadzu-6000, Cu Ka, 1.544 Å A). Particle size analyses were car-
ried out using the laser diffraction method (Malvern Mastersizer-
2000).
2.2. The preparation of the geopolymer mortar
Three different molarities (M) of NaOH concentration were used
in order to determine the effect of NaOH concentration on geopoly-
mer mortars. Dissolved NaOH pellets were used in order to obtain
concentration. The materials and the mixture proportions used in
the preparation of the geopolymer mortar samples are shown in
Table 1.
The mortars were shaped in 40 mm  40 mm  160 mm metal
molds using a vibration method. Afterwards, the samples were
placed in a laboratory-type oven to cure thermally. The curing tem-
peratures and curing times used in a study in the literature [5]
were applied to the geopolymer mortars in this study. The samples
are shown in Table 2. The samples cured at 65 °C were coded as A
and those cured at 85 °C as B. When a prepared geopolymer mortar
was activated by 3 M NaOH and cured at 65 °C for 24 h, this set of
samples was coded as 3A-24. Other mortars were also encoded
depending on NaOH concentration, curing temperature and curing
time (Table 2). Table 3 shows the initial molar ratios of SiO2, Al2O3,
Na2O and H2O of the alkali-activated fly ash paste.
2.3. Mixing procedure
NaOH was used together with sodium silicate solution to dis-
solve the silica and alumina of the fly ash particles [1]. The NaOH
solutions were prepared in the planned concentrations and al-
lowed to stand at room temperature for 24 h. Next, the fly ash
and NaOH solution were mixed for 3 min. Sodium silicate solution
was added to the mixture and mixed for another minute. Lastly,
sand was added to the mixture and mixed for 3 min. A solution
with the module 3 (SiO2/Na2O), sodium silicate (water glass) was
added to the mixtures. Table 4 shows the properties of the NaOH
and sodium silicate solution. The specific gravity of the crushed
sand used in the production of mortar was 2.27 g/cm3. The grain
size of the crushed sand used in the preparation of mortar was
2 mm at the most. Fineness modulus of the aggregate was 1.25.
2.4. Physical and mechanical tests
After the curing process, the geopolymer mortars were stored at
room temperature until physical and mechanical tests were con-
ducted. 7-day geopolymer mortar samples were used in the tests.
The average of three samples from each sample group was taken
for the physical tests and flexural strength test while the results
of the compressive strength test were determined by taking the
average of six samples.
Some of the geopolymer mortars were placed in a water tank to
determine their physical properties. The principles of Archimedes
were used to determine the physical properties of these samples
 G. Görhan, G. Kürklü / Composites: Part B 58 (2014) 371–377 373

Table 1
Mix proportion of mortars.

Concentration of NaOH (M) Fly ash (g) Sand (g) Sodium silicate solution (ml) Solution of NaOH (ml) Solid/liquid ratioa (mass) Liquid/fly ash ratio (mass)
3 450 1350 290 145 3.92 1.04
6 450 1350 290 145 4.14 1.00
9 450 1350 290 145 4.37 0.97
a
Solid included fly ash, sand and NaOH in pellet form.

Table 2
The prepared samples and curing process.

Geopolymer Concentration of NaOH Curing time Curing temperature Geopolymer Concentration of NaOH Curing time Curing temperature
(M) (h) (°C) (M) (h) (°C)
3A-2 3 2 65 3B-2 3 2 85
3A-5 3 5 65 3B-5 3 5 85
3A-24 3 24 65 3B-24 3 24 85
6A-2 6 2 65 6B-2 6 2 85
6A-5 6 5 65 6B-5 6 5 85
6A-24 6 24 65 6B-24 6 24 85
9A-2 9 2 65 9B-2 9 2 85
9A-5 9 5 65 9B-5 9 5 85
9A-24 9 24 65 9B-24 9 24 85

diffraction graph (XRD) of the fly ash obtained in a previous study

Table 3 [33], it contained quartz, magnetite, anhydrite, anorthite, hematite,
The initial molar ratios of alkali-activated fly ash paste.
and other minerals (Fig. 1). Table 6 shows d10, d50 and d90 values of
Concentration of NaOH SiO2/Al2O3 Na2O/Al2O3 H2O/Na2O the fly ash. The specific surface area was calculated as 0.366 m2/g.
3M 5.24 0.85 30.62
6M 5.24 1.36 18.87
3.2. Physical properties of the fly ash based geopolymer mortars
9M 5.24 1.86 13.47

Increases in curing time led to a reduction in apparent porosity

in the geopolymer mortars cured thermally at 85 °C. In Fig. 2b is
Table 4
show that the highest value of porosity was obtained from 3B-2
Chemical materials and their properties.
(Fig. 2b) mortars which had low NaOH concentration while the
Sodium silicate solution (water glass) Sodium hydroxide (NaOH) lowest porosity values were obtained from 3B-24 mortars. With
Na2O: 7.5–8.5 % M: 40 g/mol an increase in the curing temperature, the apparent porosity of
SiO2: 25.5–28.5 % NaOH P 97.0 the geopolymer mortars increases at 2 h of cure state onwards,
Density (20 °C) 1.296–1.396 g/ml while it decreases at 24 h of cure state. Out of the samples cured
Fe 6 0.005 %
Heavy metals: (as Pb) 6 0.005 % [28]
for 5 h, the porosity of the samples with a concentration of 6 M
and 9 M NaOH decreased with an increase in the curing tempera-
ture. In the samples cured for 2 h higher porosity was observed be-
cause the reaction was very low and provided greater evaporation
including water absorption, porosity, bulk density and apparent at 85 °C than at 65 °C, while in the samples of 5 and 24 h pores
density. TS EN 772-4 [29] was used to determine the apparent were clogged by the formed gel geopolymeric reaction (Fig. 2).
porosity, bulk density and apparent density values of the samples In addition to the curing process, NaOH solutions of different
while TS EN 771-1 [30] was used to determine the water absorp- concentration used in the preparation of the geopolymer mortars
tion values of the samples. TS EN 196-1 [31] was used to determine had an effect on the values of porosity. The samples cured at
the mechanical properties of the geopolymer mortars. 65 °C, especially the samples with 6 M NaOH concentration (6A-
2, 6A-5 and 6A-24), had a more porous structure (Fig. 2a), and
3. Results and discussion the apparent porosity ranged from 26.1% to 29.2%.
The increase in the curing times reduced the apparent porosity
3.1. Physical and chemical properties of the fly ash in the samples cured at 85 °C. These values ranged from 25.3% to
29.8%. The porosity reduced in inverse proportion to the increase
According to the results of the XRF analysis of the fly ash, the in NaOH concentration in the samples cured for shorter periods
total SiO2 + Al2O3 + Fe2O3 value of the fly ash was 80.09% while of time (3B-2, 6B-2 and 9B-2). However, this relationship was re-
the value of CaO was 6.06%. The fly ash was a Class F fly ash accord- versed with an increase in the curing time, and porosity increased
ing to ASTM C 618 [32]. The silica/alumina ratio of the fly ash by in direct proportion to NaOH concentration in the mortars cured
mass was (SiO2/Al2O3) 2.49 (Table 5). According to the X-ray for 24 h (3B-24, 6B-24 and 9B-24). The effect of the NaOH

Table 5
Chemical composition of fly ash.

Oxide SiO2 Al2O3 Fe2O3 MgO Na2O K2O SO3 CaO LOI Total
Weight,% 48.90 19.63 11.56 4.31 0.73 2.06 1.65 6.06 2.32 97.22
374 G. Görhan, G. Kürklü / Composites: Part B 58 (2014) 371–377

between 15.6% and 19.2%. When curing was carried out at 85 °C,
the curing time and concentration of NaOH was directly affected
while geopolymers cured at 65 °C had no clear trend (Fig. 3b). De-
crease in the water absorption of the samples with increase in the
NaOH concentration was also observed in the previous studies
[34,35]. It was stated in the previous studies that; lower water
absorption and apparent porosity were observed when higher al-
kali content (% Na2O) activators were used in the production of
geopolymer mortars [36,37].
The bulk density values of the samples cured thermally at 65 °C
did not vary greatly (Fig. 4a). In fact, similar results were obtained
from the geopolymer mortars cured for 2 and 5 h. It was deter-
mined that the samples cured for 24 h showed a denser structure,
however, NaOH concentration was not a very important factor. The
bulk density values of the samples cured at this temperature ran-
ged from 1577.4 to 1614.6 kg/m3.
Fig. 1. X-ray diffractogram of fly ash. In the samples cured at 85 °C, the bulk density increased with
an increase in the curing time. The bulk density of the samples
Table 6 cured at this temperature ranged from 1552.9 to 1622.7 kg/m3. It
d10, d50 and d90 values of fly ash. should be noted that 9B mortars showed a denser structure when
they were cured for 2 h while they had a lower density than 3B and
Sample d10 (lm) d50 (lm) d90 (lm)
6B when they were cured for 24 h (Fig. 4b).
Fly ash 8.103 32.829 92.778
An increase in the curing temperature increased the bulk den-
sity of the geopolymer mortars with a 3 M NaOH concentration,
concentration on the geopolymer mortar samples cured for 5 h is while the effect of the temperature was not pronounced in the
not clear (Fig. 2b). samples with a 6 M and 9 M NaOH concentration. However,
Apparent porosity values are generally correlated with water regardless of the curing temperature, it was observed that the bulk
absorption values. Therefore, the water absorption values of the density of the geopolymer mortars increased with an increase in
samples showed similarities with the porosity values (Fig. 3). The the curing times (except the 9A samples).
absorption values of the samples cured at 65 °C varied between For the bulk density, all the voids of the material
16.5% and 18.5% while those of the samples cured at 85 °C varied (open pore + closed pore) were omitted. Therefore, as can be seen

(a) (b)

Fig. 2. The apparent porosity of geopolymer mortars.

(a) (b)

Fig. 3. The water absorption of geopolymer mortars.

 G. Görhan, G. Kürklü / Composites: Part B 58 (2014) 371–377
(a)
Fig. 4. The bulk density of geopolymer mortars.
in Fig. 4b, the bulk density of 3B-2 mortars is higher than that of
6B-2 mortars although the apparent porosity of the former is high-
er than the latter. This is due to the fact that the total porosity of
6B-2 sample is higher than that of 3B-2 sample and therefore a
lower level of apparent density value was observed compared to
3B-2 sample. The apparent density of the geopolymer mortars is
shown in Fig. 5. According to the findings, the effect of the NaOH
concentration on the apparent density values is not clear. However,
the apparent density values of the mortars decrease with an in-
crease in the NaOH concentration of the samples cured at 85 °C
for 24 h. The apparent density values of the samples cured at 65
and 85 °C range from 2154.8 to 2229.9 and from 2153.6 to
2214.3 kg/m3, respectively.
3.3. Mechanical properties of the fly ash based geopolymer mortars
It is important to increase the curing temperature for the sam-
ples to gain strength quickly when higher strengths are intended to
be achieved during a shorter period of time [2]. The thermal curing
process applied for more than a few hours at high temperatures
had a positive effect on compressive strength of the material
[38]. The strengths of the samples increased as a result of the cur-
ing times and the reactions between silica and alumina in the alka-
line ions [3].
Figs. 6 and 7 show the compressive and flexural strengths of the
geopolymer mortars, respectively. According to the data; low con-
tent of Si and Al ions dissolved from the fly ash particles, and this
resulted in relatively low compressive strength values due to the
low alkaline medium of the samples cured thermally at 85 °C
and activated by 3 M NaOH (Fig. 6). It was reported that a weak
chemical reaction occurs with the use of a low alkaline solution
(a)
Fig. 5. The apparent density of geopolymer mortars.
375
(b)
[39]. The compressive strength of the samples is expected to in-
crease with an increase in NaOH concentration due to the fact that
silica and alumina are filtered more in a highly concentrated NaOH
solution [40]. The dissolution of the fly ash accelerates because
OH concentration is sufficiently high in high molarities (9 M);
however it further hinders polycondensation in the structure
[41]. Higher NaOH concentration is more effective in dissolving
fly ash particles and can result in a better geopolymerization [42].
It was observed that the samples activated with 6 M NaOH had
an ideal alkaline environment and the highest compressive
strength values compared to 9 M NaOH samples. The compressive
strength values of 21.3 MPa and 22 MPa were obtained from the
6A-24 sample cured at 65 °C and from the 6B-24 sample cured at
85 °C, respectively. The reductions in the strength values of the
samples activated with 9 M NaOH are thought to have resulted
from an increase in the coagulation of silica [1].
The flexural strength of the geopolymer mortars revealed differ-
ent trends depending on the curing temperature. In the samples
cured at 65 °C, the flexural strengths of the mortars cured for 2
and 5 h decreased with an increase in the NaOH concentration. A
different situation was observed in the mortars cured for 24 h. In
the samples cured at 65 °C, flexural strengths varied between 4.9
and 7 MPa. In the geopolymer mortars cured at 85 °C, the flexural
strengths of the samples with 3 M and 9 M NaOH concentration in-
creased with an increase in the curing time. In addition, in the geo-
polymer mortar samples with 6 M NaOH concentration (cured at
85 °C), lower flexural strength values were observed in the samples
cured for 2 h while the flexural strength values of the samples
cured for 5 and 24 h were the same. The flexural strength values
of the samples with 6 M and 9 M NaOH concentration cured at
85 °C reached higher levels than those of the samples cured at
(b)
376 G. Görhan, G. Kürklü / Composites: Part B 58 (2014) 371–377
(a)
Fig. 6. The compressive strength of geopolymer mortars.
(a)
Fig. 7. The flexural strength of geopolymer mortars.
65 °C. The flexural strength values of the samples cured at 85 °C
ranged from 5.5 to 8.1 MPa.
When the flexural and compressive strength values were eval-
uated together, it was determined that 3A-2 mortars cured at
65 °C for 2 h had higher strength values than those of other sam-
ples (6A-2 and 9A-2). The decline in the strength values with an
increase in NaOH concentrations was noticeable at this stage. It
was determined that the compressive strength values of the mor-
tars cured for 2 h varied depending on the curing temperature and
NaOH concentration [5]. Considering the samples cured at 65 °C for
24 h, the samples with a concentration of 6 M NaOH were found to
have the highest strength values (Figs. 6 and 7). In the samples
cured at 85 °C for 2 and 5 h, the samples with a concentration of
6 M NaOH had the highest strength values.
4. Conclusions
The increase in the curing times led to reductions in the poros-
ity values of the geopolymer mortars (samples except 3A and 6A)
while the concentrations of NaOH solutions used in the prepara-
tion of the geopolymer mortars affected both the porosity values
and curing process.. The bulk density values of the samples cured
at 85 °C increased with an increase in the curing time, while it
did not change substantially at 65 °C.
The samples of the seven-day geopolymer mortars which were
activated by 6 M NaOH were observed to have the optimum condi-
tion and the highest compressive strength values. When strength
values were considered the samples of the seven-day geopolymer
mortars which were activated by 6 M NaOH were observed to have
(b)
(b)
the optimum condition and the highest compressive strength
values when cured at 85 °C.
It was determined that an increase in the curing temperature
increased the compressive strength while it did not have a signif-
icant effect on the physical properties.
Acknowledgements
The authors would like to thank KOLSAN Inc. for the supply of
fly ash and sand and for their support. They would also like to
thank Afyon Kocatepe University Scientific Research Unit for pro-
viding financial support for this research (AKU BAP: 12.MUH.05).
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