Construction and Building Materials 94 (2015) 228–234

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Construction and Building Materials

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The evaluation with anova of the effect of lime admixture and thermal
cure time on fly ash paste activated with sodium silicate solution
Gökhan Görhan
Afyon Kocatepe University, Engineering Faculty, Civil Engineering Department, 03200 Afyonkarahisar, Turkey

h i g h l i g h t s

 Fly ash was activated with sodium silicate solution and quenched calcium lime.
 The samples were subjected to thermal curing at +105 °C for 12, 24 and 48 h.
 The curing time had no statistically significant effect on water absorption.
 The lime rate had no statistically significant effect on the apparent density.

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

Article history: Class F fly ash obtained from Kütahya Seyitömer (Turkey) thermal power plant was used as raw material
Received 6 January 2015 in this study. Fly ash was activated with sodium silicate solution (water glass) and quenched calcium lime
Received in revised form 3 May 2015 was substituted to the mixture at rates ranging from 10% to 30%. Then, samples were formed in
Accepted 6 July 2015
4  4  16 cm metal molds by means of the vibration method. The samples were subjected to thermal
Available online 10 July 2015
curing in a laboratory type oven at +105 °C for 12, 24 and 48 h in order for them to acquire resistance.
After the curing process, the physical properties such as apparent porosity, apparent density, bulk den-
Keywords:
sity, water absorption by weight and linear shrinkage, and the mechanical properties such as flexural
Sodium silicate solution
Fly ash
strength and compressive strength of the samples were determined by the three samples for each mix-
Lime ture. After the physical and mechanical tests, a two-factor analysis of variance (ANOVA) and a compara-
Thermal cure tive analysis of the mean values were carried out in order to investigate the effects of the variables used
in the production and the preparation of the samples on the values. Consequently, it was determined that
in the fly ash–lime mixtures, 24 h curing for the samples with 20% lime substitution is very efficient and
that these samples yield the best compressive strength.
Ó 2015 Elsevier Ltd. All rights reserved.

1. Introduction crumbled natural metamorphic rocks or kaolinite clay (metakaoli-

The geopolymerization process which generates new materials
with cement characteristics is a complex process and has been
poorly understood in detail so far [1,2]. Compared to ordinary port-
land cement (OPC), geopolymers have excellent properties such as
high compressive strength [3,4], low shrinkage [4], acid resistance
[4,5], fire endurance and no toxic fume emission, low thermal con-
ductivity [4], excellent heavy metal immobilization and high tem-
perature stability [1].
The geopolymerization process begins with the reaction of
alkali silicate and alkali salts at low temperatures with industrial
waste such as fly ash, coal slag, blast furnace slag, silica fume or
with dehydrated alumino-silicate soil solids such as volcanic tuffs,
E-mail address: ggorhan@aku.edu.tr
nit) calcined at 750 °C [6]. A geopolymer reaction starting at room
temperature is extended by subjecting it to heat treatment in an
oven or in a steam room between the temperatures of 40 and
100 °C after achieving the desired mixture. Thus, the properties
of the desired material are improved [7].
Alkaline activators have an important role in the dissolution of
Al and Si oxides in the raw material structure which will be
activated. Hence, sodium hydroxide (NaOH), potassium hydroxide
(KOH), potassium silicate or sodium silicate is the most widely
used activators for the synthesis of aluminosilicate reactive
material in the activation process [8–15]. The characteristics of
the product obtained in the activation process can vary depending
on the temperature and time of the applied heat curing or
calcination process. Alkali activation is generally described as
geopolymerization [16].

http://dx.doi.org/10.1016/j.conbuildmat.2015.07.011
0950-0618/Ó 2015 Elsevier Ltd. All rights reserved.
 G. Görhan / Construction and Building Materials 94 (2015) 228–234
Geopolymer maintains its internal reactions after it takes form
similarly to portland cement. The exothermic reaction of geopoly-
mer continues until it forms the three-dimensional oligomer
macromolecular structure. Water glass (sodium silicate)
(Na2SiO3) or gibbsite (sodium aluminate) (Na2O-Al2O3) is added
so that the main components in the fly ash dissolve together with
alkaline salt in a more regular fashion and this way, the properties
of the geopolymer material improve. Solutions to which these
chemicals are added are called solid-gel solutions. The use of a
great amount of water in such solutions for the dissolution of
chemicals reduces the compressive strength properties of the
material. The concentration of precipitate sodium ion is high in
such compositions. Nuclear magnetic resonance (NMR) shows that
sodium aluminate tetrahedral containing Al and Si, which are the
main elements of fly ash, facilitates the formation of the alu-
minium bond structure and that water glass increases the
cross-linked silicate molecules [6].
Geopolymers are generally prepared at low temperatures using
fly ash [2]. Fly ash, which is a thermal power plant solid waste, con-
tains silicon and aluminium which can be activated by alkaline
solutions [17]. Since fly ash particles are formed at high tempera-
tures, they have a chemically stable and glass-like structure.
Therefore, the reactivity in the process of hydration of fly ash is
low. Alkali activations are used to increase the pozzolanic reactiv-
ity of fly ash, and alkalis such as NaOH, Ca(OH)2 etc. are used in
these processes [18].
Liquid solution which will be used in the activation process can
be either a single material or formed by mixing a number of differ-
ent materials [17]. In the activation process, a strong alkaline med-
ium is needed to increase the surface hydrolysis of the raw
material particles with the dissolution of an amount of silica and
alumina particles in the material. This medium can be obtained
by using a single or combined alkaline solutions referred to as acti-
vators [16].
The raw material of alkaline lime is CaO and is obtained by the
sintering of CaCO3, also known as limestone, between 850 and
900 °C. Limes are not used in the form of calcium oxide (CaO).
They have to be quenched, and the quenching of the lime is a
hydration process. When quenched, the size of the lime increases
2–2.5 times. Deformation and cracks may occur in the material if
the lime containing material is not thoroughly quenched. When
hydrated lime–calcium hydroxide Ca(OH)2–(CH) is treated with
plenty of water, CH particles are dispersed in suspension in the
water [19].
Information regarding the surface of CH particles in an environ-
ment where CH is abundant is scarce in the literature. However,
one study shows that the consumption rate of CH increased in
the CH and fly ash mixtures with an increase in the content of
CH during the first mixture. The increase in the consumption rate
was accounted for by the increase in the calcium ions in parallel
with the increase of CH surfaces in the solution. Another study
states that in the case of an increase in the CH/fly ash ratio in
the starting material, the consumption rate of CH increases [20].
It is observed that in general studies on the activation of fly ash
prefer to use two different alkaline activator materials, and differ-
ent curing times and temperatures in the activation process. In one
of these studies, Thokchom et al. cured the samples produced by
using fly ash and sand at 85 °C for 48 h [21]. Rickard et al. used
sodium silicate and sodium aluminate solutions for the synthesis
of fly ash based geopolymer and cured the samples at 70 °C for
24 h [22]. Sarker used sodium hydroxide and sodium silicate in
the production of fly ash based geopolymer concrete and cured
the samples at 60 °C for 24 h. He suggested that the samples
yielded satisfactory results [23]. In addition, there are some studies
in the literature in which fly ash content geopolymer materials are
produced [24–29]. Furthermore, NaOH is a good activator for the
229
activation of fly ash. It is also stated that, due to the high Si content,
the use of water glass during geopolymerization leads to a high
mechanical resistance in samples [30]. However, the use of water
glass in the form of powder is observed to lead to lower perfor-
mance than when the liquid form is used [10].
There is little information in the literature on fly ash activated
with alkaline solution–calcium hydroxide pastes. It is pointed out
that the thermal curing of fly ash–CH containing systems at
100 °C, increases hydrate products to higher levels [20].
Therefore, different from the literature, in this study, fly ash–lime
pastes activated only with sodium silicate solution were subjected
to thermal curing at high temperatures. Ca(OH)2 substitution was
carried out for the activation process of the fly ash to be more
effective during the preparation of the pastes and then the proper-
ties of the samples were investigated. Two-factor ANOVA tests
were applied in order to determine the effects of the factors (curing
time and lime rate of substitution) on the data obtained. The
two-factor ANOVA test is a statistical method which analyses the
main effects of factors and the joint effect of two factors on a
dependent variable instead of analysing separately the effect of
two factors between groups on a dependent variable [31]. The lit-
erature includes studies in which ANOVA tests are applied [32–38].
2. Material and method
2.1. Materials
Fly ash with low levels of calcium oxide (CaO) and a SiO2/Al2O3
ratio of 2.41 by mass was used in this study as raw material
(Table 1) and it was obtained from Kütahya Seyitömer thermal
power plant. The chemical composition of the fly ash was deter-
mined by X-ray fluorescence (XRF) analysis and it is presented in
Table 1. According to the data obtained from the XRF analysis,
the fly ash was of Class F according to ASTM C-618 [39].
Fig. 1 presents the XRD graphic of the mineralogical analysis of
the fly ash. According to the XRD analysis, the main minerals in the
fly ash are quartz, magnetite, anhydride, anorthite and hematite.
S-KK 80 T quenched calcium lime, which conforms to TS 4022
[41], was used as replacement material during the production of
the samples (Table 2).
2.2. Preparation of samples
In the preparation of the samples, fly ash and lime were first dry
mixed until reaching a homogeneous state. Then, mixing water
which was equal to the sum of the mass weight of the mixture
was prepared. Accordingly, one unit of dry material was mixed
with one unit of mixing water. The mixing water was prepared
in a way that 1=4 of it was water and 3=4 of it was sodium silicate
solution (water glass) (Na2O
SiO2) by weight for all the mixtures.
Table 3 presents the prepared mixtures and the ingredients they
contain.
Through substitution, lime admixture was added to the fly ash
based mixtures activated with sodium silicate solution. After the
mixtures were homogeneously mixed, they were placed into
cement mortar molds (4  4  16 cm) with the help of a vibrating
table. Then, the samples were subjected to thermal curing in a lab-
oratory type oven at +105 °C. Three samples for each sample group
were used in the physical and mechanical tests. Three different
curing times (12, 24 and 48 h) were used in the curing of the
samples.
2.3. Tests
After the curing processes, the samples were placed in a water
tank for 24 h to determine their physical properties. Water
230 G. Görhan / Construction and Building Materials 94 (2015) 228–234

Table 1
Chemical analysis values of fly ash [40].

SiO2 Al2O3 Na2O Fe2O3 CaO MgO P2O5 SO3 K2O MnO TiO2 Cr2O3 LOI
46.30 19.20 0.51 11.00 6.34 4.76 0.10 1.54 2.45 0.11 0.87 0.12 3.26

Fig. 1. XRD graphic of Fly ash [40].

Table 2 according to TS 4790 [45]. The flexural and compressive strengths

The chemical properties of lime [42]. of the samples after curing were determined according to the TS EN
Properties S-KK 80 196-1 [46] standard.
CaO + MgO (% by mass, the least) 80
Lastly, two-factor analysis of variance (ANOVA) was carried out
MgO (% by mass) 65 in order to investigate the effects of the variables used in the pro-
CO2 (% by mass, the least) 7 duction and preparation of the samples on the values. Following
Acid-insoluble matter (including SiO2, % by mass, the least) 2 the determination of the significant differences of the factors, com-
R2O3 (metal oxides) (Al2O3 + Fe2O3) (% by mass, the least) 1
parative analysis of the mean values of the samples were carried
SO3 (% by mass, the least) 2
out in order to determine which groups showed those differences.
The confidence interval for statistical tests was 95% (a = 0.05) in
the study.
absorption, apparent porosity, bulk density and apparent density
values were determined according to Archimedes principle.
During the determination of the physical properties, the samples 3. Results and discussion
were removed from the water tank and submerged weights and
saturated surface dry weights were calculated. Then the samples 3.1. Physical properties
were dried in the oven until a constant weight was reached.
With the help of these values, the apparent porosity, apparent den- The data show that the pastes cured for 24 and 48 h yield sim-
sity and bulk density of the samples were determined according to ilar values for their physical properties. However, depending on the
TS EN 772-4 [43] and the water absorption values were deter- curing time, the intensity values of the samples cured for 12 h were
mined according to TS EN 771-1 [44]. Then, the linear shrinkage lower than those of the samples cured for 24 and 48 h. The increase
rates of the paste samples cured for 12 h were determined in curing time applied to the paste samples led to an increase in the
number of open pores. It is estimated that, during the extended
curing times, porosity ratios increase as a result of the withdrawal
Table 3 of the inert liquid in the system. Of all the samples, the highest
The mixtures and the rates of the materials they contain (%).
apparent porosity ratio (51.4%) was obtained from the C2 samples,
Mixtures Fly ash (%) Lime (%) Curing time (h) while the lowest apparent porosity ratio (43.4%) was obtained
A1 90 10 12 from the A1 samples (Fig. 2a). In addition, the effect of the lime
A2 80 20 12 substitution in the production of the samples on the porosity val-
A3 70 30 12 ues was found to be unclear and inconsistent.
B1 90 10 24 Considering the water absorption rate by weight obtained in
B2 80 20 24 relation to the apparent porosity, it was observed that the water
B3 70 30 24
absorption rate by weight of the samples ranged from 42.5% to
C1 90 10 48 51.0% and the lowest water absorption rate (42.5%) and the highest
C2 80 20 48
water absorption rate (51.0%) was obtained from C samples cured
C3 70 30 48
for 48 h. (Fig. 2b). In the mixtures with 10% lime substitution, the
 G. Görhan / Construction and Building Materials 94 (2015) 228–234
(a) 60
App. porosity
50
40
(%)
30
20
10
0 0
A1 A2 A3 B1 B2 B3 C1 C2 C3
Mixture
Fig. 2. Apparent porosity and water absorption values of the samples.
increase in the curing time increased the water absorption rates
while in the mixtures with 30% lime substitution the increase in
the curing time reduced the water absorption rates. However, the
effect of the increase in the curing time on the water absorption
rates of the mixtures with 20% lime substitution is not clear.
Furthermore, it is also reported that during the curing process,
materials are prone to high water absorption as a result of water
and alkali movement on the surface of the geopolymer material
[47].
In general, bulk density is expected to increase with a decrease
in the apparent porosity ratio. The samples produced in this study
have a similar tendency. The bulk density values of the pastes
cured for 24 and 48 h are in close proximity. However, the bulk
density values of the samples cured for 12 h were observed to be
lower than those of the samples cured for 24 and 48 h. Many stud-
ies in the literature report that the applied curing time has a signif-
icant effect on the resistance of alkali activated materials.
Therefore, it is estimated that the 12 h thermal curing applied to
the fly ash–lime pastes does not allow adequate chemical reaction
in the material and thus, the bulk density remains at lower levels
compared to the long thermal curing (Fig. 3a). The effect of the
lime admixture on the bulk density values of the samples cured
for 24 h was unclear while a linear increase in the bulk density val-
ues of the samples cured for 48 h was observed with an increase in
the lime admixture. Lime contribution to the samples cured for
12 h led to a decrease in their bulk density values. Of these sample
groups, C3 samples had the highest bulk density value of
1081.7 kg/m3 (Fig. 3a).
The apparent density values of all samples regardless of the cur-
ing time were between 1662.4 kg/m3 and 2081.1 kg/m3. Of the
(a) 1200
Bulk Density
1000
800
(kg/m3)
600
400
200
0 0
A1 A2 A3 B1 B2 B3 C1 C2 C3
Mixture
Fig. 3. Bulk density and apparent density values of the samples.
231
(b) 60
Water absorption
50
40
(%)
30
20
10
A1 A2 A3 B1 B2 B3 C1 C2 C3
Mixture
samples cured for 12, 24 and 48 h; A2, B2 and C2 samples had
the highest density. Considering the density values, we can state
that the samples with 20% lime substitution resulted in a better
microstructure for each curing time (Fig. 3b).
Linear shrinkage ratios of the fly ash–lime pastes increased with
an increase in the lime substitution ratios. Accordingly, linear
shrinkage ratios of the pastes with 10%, 20% and 30% lime substitu-
tion ratios were 1.6%, 1.8% and 2.0%, respectively.
3.2. Mechanical properties
Fig. 4 presents the flexural strength and compressive strength
values, which are two of the mechanical properties. According to
the findings, an increase in the curing time applied to the samples
led to significant changes in their resistance values. In general, the
flexural strength of the samples decreased with the prolonged cur-
ing time. It was determined that not only the curing time but also
the lime substitution ratios were effective on the reduction of the
flexural strength values. As a matter of fact, a certain level of loss in
flexural strength was observed with the increase in the amount of
lime added to the mixture. Of the 10% and 20% lime substituted
samples, the highest flexural strength values were obtained from
the pastes cured for 12 h while, of the 30% lime substituted sam-
ples, the highest flexural strength values were obtained from the
pastes cured for 24 h (Fig. 4a).
It was observed that, in contrast to the flexural strength values
of the samples cured for 12 h, they were unable to exhibit com-
pressive strength. What is more, the compressive strength ratios
of the samples cured for 12 h were observed to decrease with the
increase of the lime ratio in the mixture (Fig. 4b). Compressive
(b) 2500
App. Density
2000
1500
(kg/m3)
1000
500
A1 A2 A3 B1 B2 B3 C1 C2 C3
Mixture
232 G. Görhan / Construction and Building Materials 94 (2015) 228–234

(a) 1.4 (b) 12

Flexural Strength Compressive
1.2 10 Strength
1
8
0.8
(MPa)

(MPa)
6
0.6
4
0.4

0.2 2

0 0
A1 A2 A3 B1 B2 B3 C1 C2 C3 A1 A2 A3 B1 B2 B3 C1 C2 C3
Mixture Mixture

Fig. 4. Flexural strength and compressive strength values of the samples.

strength increased only in the samples with 10% lime substitution
with the increase in the curing time. Khatib et al. reported that a
3.5 MPa compressive strength was reached in the samples with
10% lime substitution after 56 days [48]. From this perspective, it
is clear how important the strength values obtained in the study
are.
The effect of the curing time is not clear for other substitution
rates (20% and 30%). In fact, a previous study reports that even in
the case of making preliminary improvement in the raw material,
the chemical and structural properties of minerals are complex and
yield different results [49].
Compressive strength values indicate that 24 h curing for the
samples with 20% lime substitution is very efficient and that these
samples yield the best compressive strength. It is also reported in
the literature that the strength of pozzolan–hydrated lime mix-
tures increases with an increase in the hydrated lime ratios and
that the critical rate varies between 20% and 35% [50].
3.3. Statistical analysis
A two-way analysis of variance (ANOVA) test was carried out
for the data obtained from the samples and the results were pre-
sented in Table 4. Analysis was performed combined and sepa-
rately on the resulting data, for the effect of the lime rate and
curing time. According to the analysis, the lime rate had a statisti-
cally significant effect on the apparent porosity, water absorption,
bulk density, flexural strength and compressive strength. However,
the lime rate was observed to have no statistically significant effect
on the apparent density values.
It was determined that the curing time had no statistically sig-
nificant effect on water absorption. However, it was observed that
the combined effect of the lime rate and the curing time on the
apparent porosity, water absorption, bulk density, and compres-
sive strength values of the samples was statistically significant
(Table 4).
Mean values obtained by taking the curing time into account
are presented in Table 5. Considering the mean values, it was
observed that the applied curing time had no statistically
significant effect on the water absorption values of the samples.
As a matter of fact, Table 4 indicates that the curing time, com-
pared to the ANOVA results, had an effect on apparent porosity,
bulk density, apparent density, flexural strength and compressive
strength values. In terms of mechanical properties, it can be stated
that the effect of the curing time on the compressive strength val-
ues is more pronounced. Evaluating the mean values obtained
according to the curing time and ANOVA results together, it was
observed that the compressive strength values of the samples were
at higher levels when cured for 24 h. These results are also sup-
ported by the ANOVA results. The flexural strength values were
at higher levels when the samples were cured for 12 h. The flexural
strength values of the samples cured for 12, 24 and 48 h were
0.8 MPa, 0.7 MPa and 0.5 MPa, respectively. Hence, it was observed
that the curing time did not have a statistically significant effect on
the water absorption of the samples, whilst it had a statistically
significant effect on mechanical properties such as compressive
strength and flexural strength values. As the analyses were carried
out in the 95% confidence interval for the ANOVA results, the cur-
ing time was observed to have not a statistically significant effect
only on the water absorption values.
The mean values obtained by the lime admixture rate are pre-
sented in Table 6. The water absorption and apparent porosity
rates, which are two of the physical properties of the samples, were
observed to have decreased with an increase in the lime rate. The
highest mean water absorption and apparent porosity rates were
49.0% and 48.8%, respectively for the samples with a 20% lime rate.
The apparent porosity rates which decreased with an increase in
the lime rate led to an increase in the bulk density rates of the sam-
ples and the highest bulk density (1019.3 kg/m3) was obtained
from the samples with a 30% lime rate. The mean apparent density
values tended to increase although the effect of the lime rate on the
apparent density values was unclear.
The mean flexural strength values of the samples decreased
with an increase in the lime rate. The mean flexural strength values
of the samples with a 10% lime rate and a 30% lime rate were
0.9 MPa and 0.4 MPa, respectively. The mean compressive strength
values of the samples varied depending on the lime rate and the

Table 4
ANOVA results of the values (a = 0.05).

Source of variance p Values

Apparent porosity Water absorption Bulk density Apparent density Flexural strength Compressive strength
Lime rate (L) 0.023076 0.039300 0.028562 0.088238 0.001949 1.21E 05
Curing time (T) 2.12E 05 0.340799 6.26E 08 3.44E 12 0.021911 5.8E 11
L*T 0.000217 0.000923 0.025988 0.100428 0.096207 1.21E 07
 G. Görhan / Construction and Building Materials 94 (2015) 228–234 233

Table 5
Mean values of the samples depending on curing times.

Group of Water absorption Apparent porosity Bulk density (kg/ Apparent density (kg/ Flexural strength Compressive strength
sample (%) (%) m3) m3) (MPa) (MPa)
A 48.8 45.7 935.7 1722.8 0.8 3.5
B 47.2 48.8 1033.7 2017.4 0.7 8.4
C 48.0 49.4 1033.8 2045.3 0.5 7.5

Table 6 Consequently, it was determined that in the fly ash–lime mix-

Mean values of the samples depending on the lime rate.
Lime rate 10% 20%
Water absorption (%) 48.7 49.0
Apparent porosity (%) 48.1 48.8
Bulk density (kg/m3) 985.5 998.4
Apparent density (kg/m3) 1909.4 1954.9
Flexural strength (MPa) 0.9 0.7
Compressive strength (MPa) 5.7 7.8
highest mean compressive strength value (7.8 MPa) was obtained
from the samples with a 20% lime rate.
4. Conclusion
Given the physical, mechanical and statistical findings of the
study, the results are as follows;
 No major change was observed in the physical properties of the
fly ash–lime pastes after 24 and 48 h curing times. However, the
12 h curing time reduced the density values of the samples
compared to the other samples.
 The effect of the lime substitution ratios used in the preparation
of the pastes on the physical properties such as porosity and
water absorption is varied.
 The increase in the lime substitution ratios led to an increase in
the linear shrinkage rates of the samples.
 Significant changes were observed in the resistance values of
the samples with the increase in the curing time. Accordingly,
the flexural strength of the samples decreased with the pro-
longed curing time. It was determined that it was not only the
curing time that caused the reduction in the flexural strength
values, but the lime substitution ratios were another factor for
the reduction.
 The compressive strength values increased with an increase in
the curing time for the fly ash–lime pastes with only 10% lime
substitution. The effect of the curing time on the compressive
strength varies for other substitution rates (20% and 30%).
 It was determined that the curing time had no statistically sig-
nificant effect on water absorption. However, it was observed
that the combined effect of the lime rate and the curing time
on the apparent porosity, water absorption, bulk density, and
compressive strength values of the samples was statistically
significant.
 According to the analysis, the lime rate had a statistically signif-
icant effect on the apparent porosity, water absorption, bulk
density, flexural strength and compressive strength. However,
the lime rate was observed to have no statistically significant
effect on the apparent density values.
 Evaluating the mean values obtained according to the curing
time and ANOVA results together, it was observed that the com-
pressive strength values of the samples were at higher levels
(8.4 MPa) when cured for 24 h.
 The mean compressive strength values of the samples varied
depending on the lime rate and the highest mean compressive
strength value (7.8 MPa) was obtained from the samples with
a 20% lime rate.
tures, 24 h curing for the samples with 20% lime substitution is
30% very efficient and that these samples yield the best compressive
46.3 strength.
46.9
1019.3
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