Construction and Building Materials 181 (2018) 227–237

Contents lists available at ScienceDirect

Construction and Building Materials

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

Investigating the effects of solarcure curing method on the compressive

strength, microstructure and polymeric reaction of fly ash based
geopolymer
Muhammad Zahid, Nasir Shafiq ⇑, Asif Jalal
University Technology Petronas, Malaysia

h i g h l i g h t s

Solarcure curing method is a clean technique for achieving high compressive strength of geopolymer binders.

High calcium fly ash performed better than the low calcium fly ash as the geopolymer base material.

Increasing the molarity of alkaline solution increase the compressive strength of geopolymer binders.

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

Article history: This paper presents the effects of the specially designed solarcure method on the properties of geopoly-
Received 5 March 2018 mer binders. The solarcure method is composed of the box-shaped chamber that works on the principles
Received in revised form 13 May 2018 of trapping solar radiations to regulate the adequate amount of heat and temperature inside the box. Two
Accepted 5 June 2018
sets of geopolymer binder mix containing low-calcium fly ash (LCFA) and high-calcium fly ash (HCFA) as
Available online 12 June 2018
a base material was developed. One part of sodium hydroxide (5 M and 10 M) solution mixed with two
parts of sodium silicate was used as an alkaline activator. Mortar cubes of 50 mm size were cast and
Keywords:
cured in three different regimes; continuous oven (CO) curing, intermittent oven (IO) curing and solar-
Geopolymer binder
Solarcure method
cure (SC) curing were used for the compressive strength test. For constant curing; temperature was main-
Intermittent curing tained at 60 °C 24-h, whereas in intermittent conditions (IO and SC), samples were cured in three cycles;
Fly ash each cycle was composed of 8 h curing then 16 h cooling. For IO curing, the oven temperature was main-
tained at 60 °C, however for SC curing; the solar-box chamber has achieved maximum inside temperature
up to 90 °C for each curing cycle. Specially designed SC technique caused up-to 56% increase in compres-
sive strength as compared to the compressive strength of CO cured samples. SC curing also improved the
microstructure properties and geopolymer reaction product.
Ó 2018 Elsevier Ltd. All rights reserved.

1. Introduction are formed as a result of continuous reaction occurred in alumina-

Among various construction materials, environmental impacts
of Portland cement have been debated a lot by many researchers
[12,31]. Production of one ton of Portland cement consumes 1.6
tons of raw material and 6.5 million BTUs of energy, which resulted
in approximately one-ton carbon dioxide emission [23]. Therefore,
the annual production of more than two billion tons of cement
emits a considerable amount of CO2. Researchers are making sig-
nificant efforts to change the profile of traditional concrete towards
environmental friendliness. Development of geopolymer (GP) bin-
ders is another form of high-performance concrete [15]. GP binders
⇑ Corresponding author.
E-mail address: nasirshafiq@utp.edu.my (N. Shafiq).
silica rich precursor in the presence of alkaline solution [10].
In the early development stage of GP binders, after mixing and
casting exposure to heat regime is identifies as the essential
requirement, however, developing the green heat curing condi-
tions is always discussed as the missing gap in the literature. Hard-
jito [14] observed an increase in compressive strength of LCFA
geopolymer concrete with the rise in curing temperature from
30 °C to 90 °C; the optimum curing time was obtained as 24 h.
Whereas Adam and Horianto [1] have achieved highest compres-
sive strength by curing at120 °C for 20 h, the results were obtained
by curing of samples into three different heat regimes at 80 °C, 100
°C, and 120 °C. In another research, Okoye et al. [26] used five dif-
ferent curing regimes varied from 40 °C to 120 °C at an interval of
20 °C, for 72 h, the maximum strength was achieved at 100 °C.

https://doi.org/10.1016/j.conbuildmat.2018.06.046
0950-0618/Ó 2018 Elsevier Ltd. All rights reserved.
228 M. Zahid et al. / Construction and Building Materials 181 (2018) 227–237
Memon et al. [20] developed self-compacting geopolymer con-
crete; the maximum strength was obtained using curing regime
of 70 °C for 48 h. Through a wide range of research on GP binders,
it is mostly accepted that the increase in curing temperature and
time accelerates the rate of reaction and decreases the early set
time, which often caused the enhancement of mechanical proper-
ties [27,29]. Outcomes of the previous research studies summa-
rized that GP binders achieved high compressive strength when
curing temperature was maintained 60 °C to 120 °C and the curing
period was prolonged from 20 to 72 h, which may be questioned
from sustainability viewpoints if the source of heat is non-
renewable.
Solar is a natural source and identified as the renewable form of
energy. Therefore, to answer the question of sustainability regard-
ing heat curing, solar energy can be the possible input of a dedi-
cated heat curing system for geopolymer binders. During last
two decades, successful efforts have been made in developing solar
ovens for domestic purposes [24,17]. The principal aim of this
research study was to develop environmental friendly curing
regime for producing high-performance GP matrix. Mahavar
et al. [19] have designed a box-shaped solar oven capable of
achieving inside temperature of 90 °C within 4 h duration; it traps
solar radiation and works on the greenhouse mechanism. Referring
to the concept of the solar box of Mahavar et al. [19] a solarcure
(SC) technique was designed and used in this research study for
heat curing of geopolymer binders. To investigate the effects of
SC technique on the properties of GP matrix; two other curing
regimes called continuous oven (CO), and intermittent oven (IO)
was also used for comparison. For comparative analysis, effects
on compressive strength development as well as their microstruc-
tures were investigated.
2. Materials and methods
2.1. Material properties
Two types of fly ash LCFA and HCFA obtained from local sources in Malaysia was
used as base material for this research. LCFA was acquired from Tanjung Bin 21,00
MW coal-fired power plant located in Johor, Malaysia, while HCFA was collected
from the Manjung power plant, Perak, Malaysia. Elemental composition, loss on
Table 1
Elemental composition, loss on ignition (LOI) and surface area of fly ashes.
Chemical composition of fly ash
SiO2 Al2O3 Fe2O3 CaO MgO
LCFA (%) 50.8 19.6 10.4 8 0.753
HCFA (%) 34.5 11.8 23.6 19.0 2.27
a) LCFA
Fig. 1. Micrographs of fly ashes (arrows pointing Conglomerates).
ignition (LOI) and surface area of the two sources of fly ash were determined using
X-ray fluorescence (XRF) and Brunauer Emmet Taller (BET) method; the results are
given in Table 1. Both types of fly ashes showed almost similar surface area. How-
ever, it is well noted that the CaO content was more than 10% of the total oxides in
case of HCFA. Further, the summation of the amount of SiO2, Al2O3, and Fe2O3 was
less than 70%. Hence the acquired fly ash fulfilled the classification requirements of
high calcium fly ash as per ASTM 618-10. Furthermore, Si/Al ratio of HCFA was cal-
culated as 2.49; whereas, it was measured 2.22 in case of LCFA. Fig. 1 shows the
micrograph of LCFA and HCFA samples used in this study. The samples were char-
acterized using variable pressure field emission scanning electron microscope
(model; VPFESEM Zeiss, supra55 VP). Silica sand with a maximum particle size of
710 mm and fineness modulus of 2.04 was used as aggregates; gradation is given
in Table 2. Mineralogy of micro silica sand, LCFA and HCFA were examined by X-
ray diffraction (XRD) using Siemens D 501 diffractometer. Fig. 2 is showing that
the silica sand was pure quartz (ICSD: 98-016-2490), and no other mineral was
found. Mullite (ICSD: 98-009-9328) and quartz were observed in LCFA, whereas
HCFA consisted of calcium, sodium, aluminum, silicon oxide (ICSD: 98-010-0222),
hematite (ICSD: 98-015-4192), iron nitrate (ICSD: 98-004-4612) and quartz.
Sodium hydroxide (NaOH) with 99% purity in mixed with sodium silicate (Na2Sio3)
was used as an alkaline solution to develop geopolymer reaction.
2.2. Fabrication of solarcure chamber
Solarcure (SC) chamber works on the principle of trapping solar radiation to
regulate the inside temperature [11]. In the first step; a 3-D frame with the trian-
gular arch at the top to support box-top was fabricated, the inclination angle of
the head was kept 30°. After manufacturing the 3-D structure, 12 mm thick thermo-
col sheets were pasted on the outer walls of the frame, which can maintain an inter-
nal temperature of for the long duration and aluminum foil was applied at the inner
walls of the box; it can facilitate the solar radiation within the chamber and
increase the internal temperature. For avoiding the effects of rain, the outer side
of thermocol was laminated with plastic sheets. Bubble wrap was used to make a
pad for the solar box. SC chamber was placed at 04°230 1300 N latitude and 100°58-
0
2300 E longitude with the inclined phase in southern direction refer to Fig. 3. No
solar tracking was considered, and the solar box was left in one direction (south)
during the whole curing period. Chromel alumel 6 mm Stripped Lead thermocouple
(temperature range 50 °C–+200 °C with a ±0.75 °C accuracy) were used to mea-
sure the surface temperature of geopolymer cubes. For measurement of inside air
temperature of the solar box as well as ambient and external air tempera-
ture,100 mm length K type probe with temperature measuring range from 50 °C
to +900 °C with maximum error only ±0.75 °C were used.
3. Experimental program
Twelve GP mortar mixes were prepared; the details of mix pro-
portion (by weight) are shown in Table 3. Effects of three curing
Average BET surface area
K2O SO3 TiO2 P2O5 LOI m2/g
2.32 0.596 2.41 2.02 0.6 0.9985
2.08 1.49 1.46 1.27 2.8 1.0812
b) HCFA
 M. Zahid et al. / Construction and Building Materials 181 (2018) 227–237
Table 2
Gradation of silica sand.
Sieve size (mm) 710 600 300
Passing (%) 99.8 78.12 16.14
techniques termed as CO, IO and SC were studies on the compres-
sive strength and the microstructures of samples made of 12
mixes. Before doing the mixing job, NaOH solution was prepared,
for producing one liter NaOH solution of 5 M and 10 M concentra-
tion, 200 g and 400 g of NaOH pellets were dissolved in tap water
respectively. Since the dissolution of NaOH pellets in water is an
exothermic process, therefore, the prepared solution was first
allowed to cool down before mixing. The mixing was performed
using Hobart mixture; in the first step, fly ash and sand were dry
blended for thirty seconds in slow mode, then the alkaline solution
was gradually added. After adding all chemical solution, the wet
mixing was done in the fast mode for 4 min. After complete mix-
ing, workability test was performed, which followed the require-
ments of ASTM C1437-15 standard. Finally, the mortar was
poured into the 50  50  50 mm standard cube molds; the spec-
imens remained in the mold for 24 h under ambient laboratory
conditions. The mixing of mortar and casting of cubes followed
the ASTM-C109-10.
3.1. Curing of specimens
Three curing conditions; continuous oven (CO), intermittent
oven (IO), and solarcure (SC) were applied to all mortar cube sam-
ples. In all three conditions, the full curing time was kept to 24 h. It
has been discussed by Mustafa Al Bakri et al. [22], Sumajouw [28]
and Hardijito (2005) that in case of oven curing, 60 °C was found as
the optimum temperature to achieve the maximum compressive
strength. Before putting in the SC chamber, all mortar samples
were wrapped in thin plastic sheets to avoid excessive water loss.
For taking the full advantage of daylight for SC, it was performed
intermittently. Intermittent curing (SC and IO) was done into three
cycles; each of the cycles was comprising of 8-h heat curing and
16-h cooling in the ambient condition. Atisß et al. [2], observed that
the curing of geopolymer below the temperature of 45 °C did not
contribute to the compressive strength development even if the
curing time reached to a period of 72 h. Hence, the temperature
lower than 45 °C was not considered as the proper heat curing
temperature. In this case, monitoring of the temperature of SC
Q = Quartz
Mu = Mullite
Fe = Iron nitrate
He = Hemate
Ca = Calcium sodium
alluminium silicon oxide
0 10
Fig. 2. X-ray diffraction (XRD) of HCFA, LCFA and Micro silica sand.
229
150
1.23
Fig. 3. Solarcure Curing (SC) chamber.
chamber for 8-h confirmed that the average temperature inside
the chamber was more than 45 °C. Therefore, to achieve 24 h heat
curing in case of intermittent curing, three cycles of curing were
selected.
3.2. Thermal performance of solarcure (SC) chamber
Fig. 4 shows the temperature variation of ambient air, external
air, SC chamber internal air and geopolymer samples cured in SC
chamber during each curing cycle, moreover, these results are
accompanied by the variation of the solar radiations. Three inter-
mittent curing cycles performed over three consecutive days (i.e.,
20–22 September 2016). Average of maximum ambient air tem-
perature and maximum external air temperature during three days
of intermittent curing cycles was observed between 32 °C and 40
°C. Using the perioding monitoring of the internal temperature of
SC chamber, the average was obtained at 89 °C, which was 178%
greater than the ambient air temperature. As shown in Table 4
and Fig. 4, during first curing cycle, the cloudy outdoor conditions
occurred after 2:00 pm, so the rise in temperature was observed
before that, and the decrease in temperature was noted afterward.
Therefore, the total curing time for first curing cycle was 7.5 h. It is
noticed from Fig. 4 that even during the cloudy day, the internal air
temperature of SC chamber did not decrease abruptly, which was
because of thermal insulation of thermocol. Similarly, the curing
time of 9.5 h was observed during second curing cycle and 7 h
for third curing cycle. Even during the period of passing clouds,
Q
Q Micro silica sand
Q Q Q
Q
Q
Q Mu Mu Mu Q LCFA
Mu
Q Ca He Fe HCFA
20 30 40 50 60
2 (degree)
230 M. Zahid et al. / Construction and Building Materials 181 (2018) 227–237

Table 3
GP Mortar Mix proportions.

Mix no. Group Mix designation LCFA HCFA Sanda Alkaline activatora Na2Sio3 /NaOH NAOH (concentration) W/GP solidb Curing
1 LM1 LM1N 1 – 0.5 0.45 2 5M 0.25 COc
2 LM1 LM1O 1 – 0.5 0.45 2 5M 0.25 IOd
3 LM1 LM1S 1 – 0.5 0.45 2 5M 0.25 SCe
4 LM2 LM2N 1 – 0.5 0.45 2 10 M 0.22 CO
5 LM2 LM2O 1 – 0.5 0.45 2 10 M 0.22 IO
6 LM2 LM2S 1 – 0.5 0.45 2 10 M 0.22 SC
7 HM1 HM1N – 1 0.5 0.45 2 5M 0.25 CO
8 HM1 HM1O – 1 0.5 0.45 2 5M 0.25 IO
9 HM1 HM1S – 1 0.5 0.45 2 5M 0.25 SC
10 HM2 HM2N – 1 0.5 0.45 2 10 M 0.22 CO
11 HM2 HM2O – 1 0.5 0.45 2 10 M 0.22 IO
12 HM2 HM2S – 1 0.5 0.45 2 10 M 0.22 SC
a
Quantity in mass ratio of fly ash.
b
Represents water to geopolymer solids ratio. Where ‘‘GP solids” are all the solids in NaOH and Na2SiO3 solution plus fly ash.
c
Continues oven curing.
d
Intermittent oven curing.
e
Intermittent solarcure technique.

ambient air External air SC internal air

100 1250
geopolymer sample solar radiaons

Solar radiation (W/m2)

Temperature ( C)

80 First curing day 1000

60 750
40 500
20 250
0 0
7:00 AM 9:24 AM 11:48 AM 2:12 PM 4:36 PM 7:00 PM

100 1250

Solar radiation (W/m2)

Second curing day
80 1000
Temperature ( C)

60 750
40 500
20 250
0 0
7:00 AM 9:24 AM 11:48 AM 2:12 PM 4:36 PM 7:00 PM

100 1250
Solar radiation (W/m2)

Third curing day

Temperature ( C)

80 1000

60 750

40 500

20 250

0 0
7:00 AM 9:24 AM 11:48 AM 2:12 PM 4:36 PM 7:00 PM
Time

Fig. 4. Temperature variation of ambient air, external air, SC internal air and geopolymer samples cured in SC for each curing day.

Table 4
the maximum internal air temperature of SC chamber for all three
Sky conditions, day status and curing time for each curing cycle for SC chamber. curing cycles went up to 90 °C. The gradual rise in geopolymer sur-
face temperature was noticed during every curing cycle. Direct
Curing Sky Day status Curing
cycle conditions time (h)
solar radiation increases internal air temperature as well as the
temperature of moisture content present in geopolymer samples.
First Mostly Passing clouds before 2 pm fully 7.5
cloudy cloudy eventually
This synergic effect resulted in higher peak temperature on the
Second Partly Passing clouds 9.5 surface of the sample as compared to the internal air temperature
cloudy of SC chamber. Average of peak surface temperature for all three
Third Mostly Passing clouds 7 cycles was found as 96 °C, which was 8% higher than the average
cloudy
peak internal air temperature.
 M. Zahid et al. / Construction and Building Materials 181 (2018) 227–237
Fig. 5 shows the temperature profile obtained during intermit-
tent curing using solarcure and oven curing. Geopolymer mortar
mixes were cast under lab-controlled conditions at the tempera-
ture of 23 °C, after casting, samples were left in the lab for 24
h. After 24 h, one group of samples were transferred to an oven,
and the other group was moved to SC chamber for curing. At the
end of each curing cycle, three cubes from each mix were taken
out and left in the lab for 16 h then tested for compressive
strength.
3.3. Experimental testing of hardened mortar samples
Compression test of geopolymer mortar cubes was performed
according to American standard ASTM C109-10, gradually applied
loading rate was maintained at 3.0 kN/s until the complete failure
of the sample. Elemental analysis of geopolymer mortar was per-
formed by X-ray diffraction (XRD) technique using Siemens D
501 diffractometer. Fourier transform infrared spectroscopy (FTIR)
is an infrared spectroscopy method used to identify organic, poly-
meric, and in some cases, inorganic materials. Whereas,
microstructure was studied using variable pressure field emission
scanning electron microscope by ASTM C1723-15.
4. Results and discussions
4.1. Workability of geopolymer mortar
Workability is the characteristic of freshly mixed concrete that
estimates the efforts needed to place and cast concrete without
any loss of its homogeneity. Quantitative measurement of worka-
bility usually refers to the slump flow of the mix. It has been
observed that physical properties of fly ash particles have consid-
erable influence on the slump flow of geopolymer mortar. From
the Fig. 6, it can be seen that geopolymer (GP) mortar synthesized
with low calcium fly ash (LCFA) possesses relatively lower values
of slump flow when compared to HCFA based GP mortar. Referring
to Fig. 1(a) of the SEM image of LCFA, some conglomerates, and pal-
let like particles are identified, which resist the rolling of spherical
particles when flowing in the form that reduced workability. On
the other hand, as shown in Fig. 1(b), only spherical particles were
observed in HCFA, which mobilized the rolling of particles during
pouring and placing with higher workability. Chindaprasirt and
Chareerat [6] also found that the shape of fly ash particles signifi-
cantly affects the workability of the mix. Furthermore, a decrease
in slump flow was observed with the use of higher concentration
of NaOH solution; this could be happened due to the reduction
of water to geopolymer solids ratio, the same was reported by
Chindaprasirt et al. [7]. The minimum limit of slump flow for best
workable mix was proposed as 110 ± 5% [8]. Fig. 6 shows all the
solarcure curing chamber temperature"
100
80
Temperature ( C)
60
40
20
0
Hours 0 24
Days 0 1
Fig. 5. Temperature profile of intermittent solar and intermittent oven curing.
231
LCFA HCFA
160
140
Flow (%)
120
100
5M 10 M
NaOH molarity
Fig. 6. Flow of geopolymer mortar.
mixes of this research work were able to achieve workable flow,
i.e., higher than the said limit.
4.2. Effect of curing conditions on compressive strength of geopolymer
mortar
Curing technique (usually time and temperature) largely influ-
ences the compressive strength development of geopolymer bin-
ders. Compressive strength results of GP mortar after the
completion of each curing cycle are presented in Figs. 7 and 8.
Fig. Seven is plotted to compare the effects of IO and SC curing con-
ditions on the compressive strength of GP mortar made of LCFA,
whereas, Fig. 8 is drawn to compare the results of HCFA mortar
subjected to IO and SC curing conditions. In both the cases (LCFA
and HCFA), the highest compressive strength was achieved of the
samples submitted to SC curing condition. Fig. 9 is presenting the
comparison of the effects of three curing conditions (CO, IO, and
SC) on the compressive strength. To further elaborate on the com-
parative analysis, the compressive strength of samples cured in IO
and SC conditions are benchmarked against the compressive
strength of samples cured in CO condition, for which the relative
strength is considered as unity, the results are presented in Table 5.
For comparing the effects of low calcium and high calcium fly ash
on compressive strength as drawn in Fig. 9, it is found that HCFA
performed better than LCFA. In case of HCFA matrix, high calcium
content plays a vital role in the strength development, which
exhibited cementing and pozzolanic characteristics. Hence, it helps
to gain compressive strength [13]. Furthermore, the higher Si/Al
ratio of HCFA is one of the reasons for the higher compressive
strength of HCFA based geopolymer mortar. Duxson el al. (2007)
also observed the same behavior of geopolymer with the increase
in Si/Al values. Atisß et al. [2] concluded that the strength of
geopolymer enhances with the increase in the concentration of
45 C intermient oven curing temperature
48 72 96
2 3 4
232 M. Zahid et al. / Construction and Building Materials 181 (2018) 227–237

LM1O LM2O LM1S LM2S the alkaline solution. A similar trend was observed for all GP mixes
100 of this research work; however, the rate of gain of compressive
Compressive strength (MPa)

strength was different for all combinations, please refer to Fig. 9.

80 The compressive strength was increased by 30.17%, 31.64% and
26.45% when the NaOH concentration for LCFA based geopolymer
60 was changed from 5 M to 10 M for samples cured with O, IO and
IS respectively; however, this increment was only 15.76%, 20.67%
40 and 25% for HCFA. Hence, HCFA based GP showed less sensitivity
to NaOH concentration. It could be happened because of additional
20 cementitious properties of HCFA. While considering the compres-
sive strength of CO cured sample as unity, the effect of curing
0 cycles on the compressive strength of GP mortar is given in Table 5.
1 2 3 LCFA mixes (M1 & M2) gained lower compressive strength after
Curing cycles first curing cycle than the compressive strength of M3 & M4 mixes
(HCFA). Li et al. [18] reported the similar characteristics of LCFA
Fig. 7. Compressive strength development of LCFA based geopolymer subjected to
and HCFA based GP matrix. Whereas at the completion first curing
three curing cycles.
cycle of samples subjected to SC condition, samples gained almost
100% of the compressive strength of the samples cured in CO con-
dition, which can be considered an excellent achievement of the
HM1O HM2O HM1S HM2S
solarcure chamber. Similarly, the improvement in compressive
100 strength development was observed after the completion of sec-
Compressive strength (MPa)

ond and third curing cycles.

80
4.3. Characterization of the reaction product (polymerized paste)
60

40 4.3.1. X-Ray diffraction (XRD)

Crystallographic structure and elemental analysis of the reac-
20 tion product (polymerized paste) was examined using X-Ray
diffraction (XRD) method as shown in Figs. 10 and 11. Results indi-
0 cate the presence of polycondensation of alumina-silicates in fly
1 2 3 ash that produced sodium-poly-sialate-silex (Na-PSS), which is
considered as the principal component of geopolymerization.
Curing cycles
Na-PSS is amorphous to semi-crystalline in nature. Davidovits &
Fig. 8. Compressive strength development of HCFA based geopolymer subjected to Quentin [9] highlighted that filler could be added to introduce
three curing cycles. crystallinity in geopolymer. Therefore, in this research micro-
98
85.17

100
78.46

69.87

90
67.49
67.35
Compressive strength (MPa)

80
56.17

58.2

57.9
58.3

70
43.15

44.21

60
50
40
30
20
10
0
LM1 LM2 HM1 HM2
connues oven (CO) intermient oven (IO) solarcure (SC)

Fig. 9. Compressive strength development of geopolymer mortar subjected to different curing conditions.

Table 5
Effect of curing cycles on the compressive strength of GP mortar.

Group Continues oven (CO) curing Intermittent oven (IO) curinga Solarcure (SC) curinga
1st cycle 2nd cycle 3rd cycle 1st cycle 2nd cycle 3rd cycle
LM1 1 0.42 0.88 1.02 0.93 1.27 1.56
LM2 1 0.59 0.94 1.04 1.04 1.38 1.51
HM1 1 0.63 0.85 1.01 1.00 1.22 1.35
HM2 1 0.76 0.96 1.03 1.01 1.35 1.48
a
Relative changes in compressive strength w.r.t the unit compressive strength of GP mortar cured in CO curing condition.
 M. Zahid et al. / Construction and Building Materials 181 (2018) 227–237 233

silica sand was used as filler that enhanced the crystallinity in the
matrix as observed in XRD examination. Principal peaks were
detected at 2H of 21°, 27°, 40°, 50° and 60°, which is the indicator
of the crystalline quartz content. In addition to quartz, mullite was
also present in LCFA based samples, however, whereas, iron and
calcium silicate hydrate (C–S–H) were observed in HCFA based
samples. Furthermore, higher Si/Al ratio of HCFA caused by the
improved crystallinity of the geopolymer product. Curing condi-
tions remarkably influence the formation of the crystalline struc-
ture; curing at higher temperature can change the reaction
matrix from amorphous to semi-crystalline state that results in
higher compressive strength [16]. For comparing the effects of cur-
ing techniques; high-intensity peaks of quartz were observed in all
samples subjected to SC curing technique. As given in Tables 6 and
7, by increasing the molarity of alkaline solution from 5 M to 10 M,
the increment in the quartz peak intensity was observed, which

Q
Q = Quartz
M = Mullite

Q
Q
Counts

M Q
LM2S M M Q Q Q
M Q Q Q

LM1S

LM2O

LM1O

0 10 20 30 40 50 60
2 (degree)

Fig. 10. XRD patterns of LCFA based geopolymer mixes cured with IO and SC curing techniques.

Q
Q = Quartz
I = Iron
C = Calcium silicate hydrate

Q
Q
Counts

HM2S C Q
C Q Q Q QI Q Q

HM1S

HM2O

HM1O

0 10 20 30 40 50 60
2 (degree)

Fig. 11. XRD patterns of HCFA based geopolymer mixes cured with IO and SC curing techniques.

Table 6
Quartz peak intensity of LCFA geopolymer.

Mix ‘‘Quartz” Count at 2h of

21° 27° 40° 50° 60°
LM1O 779 2301 204 309 241
LM2O 1011 2441 277 365 545
LM1S 1204 4387 832 1801 612
LM2S 2199 4498 860 1911 1011
234 M. Zahid et al. / Construction and Building Materials 181 (2018) 227–237

Table 7
Quartz peak intensity of HCFA geopolymer.

Mix ‘‘Quartz” Count at 2h of

21° 27° 40° 50° 60°
HM1O 613 3404 372 311 205
HM2O 981 3493 398 518 285
HM1S 1495 3902 567 765 672
HM2S 1612 4001 645 1053 723

LM2S

LM1S
Transmiance (%)

LM2O

LM1O

400 1000 1600 2200 2800 3400 4000

Wavenumber (cm-1)

Fig. 12. FTIR spectra of LCFA based geopolymer cured with IO and SC curing techniques.

HM2S

HM1S
Transmiance (%)

HM2O

HM1O

400 1000 1600 2200 2800 3400 4000

Wavenumber (cm-1)

Fig. 13. FTIR spectra of HCFA based geopolymer cured with IO and SC curing techniques.

Table 8
Comprehensive data of FTIR spectral peaks of LCFA geopolymer.

Mix Transmittance peak at approximately 1010 Transmittance peak at approximately 780 Transmittance peak at approximately 470
cm1 cm1 cm1
Wave number (cm1) Transmittance (%) Wave number (cm1) Transmittance (%) Wave number (cm1) Transmittance (%)
LM1O 1024.1 15.2 777.8 28.2 476.8 32.7
LM2O 1014.6 8.1 777.1 19.1 468.6 30.5
LM1S 1018.9 7.9 777.4 36.4 478.1 31.4
LM2S 1012.5 5.2 776.9 34.5 476.9 29.9

was the cause of higher compressive strength. Hawa et al. [16] and
A.M. Mustafa Al Bakri et al. [21] reported the similar findings.
4.3.2. Fourier transform infrared (FTIR) spectroscopy analysis
Fig. 12 and 13 present the FTIR spectra of LCFA and HCFA based
matrix samples cured in IO and SC conditions. FTIR was performed
to identify the polymeric compounds in the reaction product, the
hump at 470 cm1 represents the in-plane Si-O and Al-O link-
ages. Further, the band at 790 cm1 indicates the bending vibra-
tion of Si–O–Si [3,4]. Peaks at 1010 are the sign of asymmetric
vibration of Si–O–Si and Si–O–Al, which is the benchmark of
geopolymerization reaction [30]. The intensity of the bands at
 M. Zahid et al. / Construction and Building Materials 181 (2018) 227–237 235

Table 9
Comprehensive data of FTIR spectral peaks of HCFA geopolymer.

Mix Transmittance peak at approximately 1010 Transmittance peak at approximately 780 Transmittance peak at approximately 470
cm1 cm1 cm1
Wave number (cm1) Transmittance (%) Wave number (cm1) Transmittance (%) Wave number (cm1) Transmittance (%)
HM1O 1009.89 55.2 777.3 67.4 476.5 69.8
HM2O 1007.1 47.6 777.8 58.32 468.7 62.3
HM1S 1007.6 34.2 777.2 85.1 477.8 97.8
HM2S 1005.2 32.5 776.8 80.1 476.9 93.7

Fig. 14. Micrographs of LM1 (5M NaOH, LCFA), LM2 (10 M NaOH, LCFA), HM1 (5M NaOH, HCFA) and HM2 (10 M NaOH, HCFA) cured with IO and SC curing techniques.

470 cm1, 790 cm1, and 1010 cm1 represent the degree of
geopolymerization [3,4]. The intensity of the peaks mentioned
above is the indicator of the strength of geopolymer reaction;
stronger the peak represents the length of aluminosilicate chain.
It is noticed that by increasing the NaOH molarity from 5 M to
10 M, peak intensity increased. Hence, it is another justification
for achieving the higher strength by increasing the concentration
of the alkaline solution. Further, it is also observed that hump at
1010 cm1 is shifted toward lower wavenumber by increasing
the molarity of NaOH, which is the indication of the higher degree
of geopolymerization, same was also reported by Chen et al. [5].
Furthermore, the improved polymeric reaction was observed for
HCFA GP which holds higher Si/Al ratio.
Interpretation of FTIR spectral peaks of LCFA and HCFA based
matrix is presented in Tables 8 and 9, respectively. A smaller value
of transmittance is the indication of steep peak intensity. It was
236 M. Zahid et al. / Construction and Building Materials 181 (2018) 227–237
observed that by increasing NaOH molarity, both wavenumber and
transmittance at the wavenumber of 1010 cm1 shifts toward the
lower value. Curing techniques are seen to have much influence on
the structural evolution of geopolymer samples. Geopolymer cured
with IO and SC curing method showed a significant difference in
FTIR spectral peaks. The steep peak at 1010 cm1 is observed in
all samples cured with SC curing technique. Further, the wave-
length is shifted towards the lower value. Hence, it is concluded
that the optimum curing condition is SC curing method. Another
strong peak at 1450 cm1 is observed for all HCFA based mix
designs, which represent the carbonate bond. This band is consid-
ered as the benchmark for calcium silicate hydrate (C–S–H) forma-
tion in calcium-containing base material geopolymer [25]. Humps
at 1650 cm1 and 3450 cm1 were found for all geopolymer
samples; these indicate H–O–H is bending and –OH stretching
respectively, similar peaks were observed in geopolymer matrix
examined by Bakharev [3,4].
4.3.3. FESEM results
Micrographs of all eight mixes are shown in Fig. 14, reacted fly
ash and some portion of unreacted or partially reacted fly ash pre-
sented in all samples. However, the status of fly ash particle
depends on the degree of geopolymerization. Denser particle pack-
ing, and profoundly reacted fly ash are the promising components
for the strength development in geopolymers. Previous studies
revealed that increasing the concentration of alkaline solution
stimulate the reaction with the base material, which results in den-
ser particle packing [21]. Same results were observed for LCFA as
well as HCFA based geopolymer mortars.
Solarcure (SC) conditioned samples showed improvement in
the degree of geopolymerization for all mix designs, little-
unreacted fly ash particles were found in SC cured samples as com-
pared to IO cured. Denser particle packing with a higher amount of
reacted fly ash particles was found for HCFA based geopolymer
with 10 M NaOH. However, the extent of reaction was greater in
SC cured samples.
5. Conclusions
Based on experimental results, following conclusions are made:
1. Specially designed solarcure (SC) chamber managed to achieve
and maintain internal air temperature up to 90 °C, which is the
reason for its extraordinary performance towards geopolymer
(GP) curing.
2. Intermittent curing techniques (IO and SC) caused significant
improvement in achieving better compressive strength and
microstructural characteristics of GP matrix. Samples cured in
solarcure chamber showed more than 50% higher compressive
strength as compared to the samples subjected to continuous
oven curing.
3. High calcium content in HCFA improved compressive strength
and microstructures due to the presence of extra C–S–H chain.
Similarly, the compressive strength of samples was improved
by increasing the molarity of sodium hydroxide from 5 M to
10 M.
4. Improvement in compressive strength, polymeric reaction, and
microstructures associated with an increase in Si/Al of fly ash.
5. Solarcure technique caused tremendously better results as
compared to other methods for improving the crystallinity
and degree of geopolymerization, and SC resulted in less unre-
acted particles.
This paper shows that solar heat can be a potential source for
the curing of geopolymer mortar, it reduces excessive resource uti-
lization, produces high strength geopolymer with improved
microstructural properties.
6. Conflict of Interest
There is no conflict of interest in this manuscript.
Acknowledgment
The authors would like to acknowledge the University Tekno-
logi Petronas for providing the financial support to accomplish this
research study. Acknowledgment is also extended the supporting
staff of concrete technology staff for their full technical support
provided for preparation and testing of specimens.
References
[1] A.A. Adam, Horianto, The effect of temperature and duration of curing on the
strength of fly ash based geopolymer mortar, Procedia Eng. 95 (2014) 410–414,
https://doi.org/10.1016/j.proeng.2014.12.199.
_
[2] C.D. Atisß, E.B. Görür, O. Karahan, C. Bilim, S. Ilkentapar, E. Luga, Very high
strength (120 MPa) class F fly ash geopolymer mortar activated at different
NaOH amount, heat curing temperature and heat curing duration, Constr.
Build. Mater. 96 (2015) 673–678, https://doi.org/10.1016/
j.conbuildmat.2015.08.089.
[3] T. Bakharev, Geopolymeric materials prepared using Class F fly ash and
elevated temperature curing, Cem. Concr. Res. 35 (2005) 1224–1232, https://
doi.org/10.1016/j.cemconres.2004.06.031.
[4] T. Bakharev, Resistance of geopolymer materials to acid attack, Cem. Concr.
Res. 35 (2005) 658–670, https://doi.org/10.1016/j.cemconres.2004.06.005.
[5] L. Chen, Z. Wang, Y. Wang, J. Feng, Preparation and properties of alkali
activated metakaolin-based geopolymer, Mater. (Basel). 9 (2016) 1–12, https://
doi.org/10.3390/ma9090767.
[6] P. Chindaprasirt, T. Chareerat, High-strength geopolymer using fine high-
calcium fly ash, J. Mater in Civil Eng. 23 (2010) 264–271, https://doi.org/
10.1061/(ASCE)MT.1943-5533.0000161.
[7] P. Chindaprasirt, T. Chareerat, V. Sirivivatnanon, Workability and strength of
coarse high calcium fly ash geopolymer, Cem. Concr. Compos. 29 (2007) 224–
229, https://doi.org/10.1016/j.cemconcomp.2006.11.002.
[8] P. Chindaprasirt, S. Homwuttiwong, V. Sirivivatnanon, Influence of fly ash
fineness on strength, drying shrinkage and sulfate resistance of blended
cement mortar, Cem. Concr. Res. 34 (2004) 1087–1092, https://doi.org/
10.1016/j.cemconres.2003.11.021.
[9] J. Davidovits, S. Quentin, GEOPOLYMERS Inorganic polymerie new materials, J.
Therm. Anal. 37 (1991) 1633–1656.
[10] P. Duxson, S.W. Mallicoat, G.C. Lukey, W.M. Kriven, J.S.J. Van Deventer, The
effect of alkali and Si/Al ratio on the development of mechanical properties of
metakaolin-based geopolymers, Colloids Surfaces A Physicochem. Eng. Asp.
292 (2007) 8–20, https://doi.org/10.1016/j.colsurfa.2006.05.044.
[11] R. Embong, N. Shafiq, A. Kusbiantoro, M.F. Nuruddin, Effectiveness of low-
concentration acid and solar drying as pre-treatment features for producing
pozzolanic sugarcane bagasse ash, J. Clean. Prod. 112 (2016) 953–962, https://
doi.org/10.1016/j.jclepro.2015.09.066.
[12] E.G.A. Ferreira, F. Yokaichiya, M.S. Rodrigues, A.L. Beraldo, A. Isaac, N. Kardjilov,
M.K.K.D. Franco, Assessment of Greener Cement by employing thermally
treated sugarcane straw ashes, Constr. Build. Mater. 141 (2017) 343–352,
https://doi.org/10.1016/j.conbuildmat.2017.03.022.
[13] X. Guo, Metakaolin-, fly ash- and calcium hydroxide-based geopolymers :
effects of calcium on performance, Adv. Cem. Res. 27 (2015) 559–566, https://
doi.org/10.1680/adcr.14.00081.
[14] D. Hardjito, Studies of fly ash-based geopolymer concrete, Ph. D. Curtin Univ.
Technol. Dept. Civ. Eng., 2005, http://espace.library.curtin.edu.au/cgi-bin/
espace.pdf?file=/2008/09/16/file_1/18580.
[15] D. Hardjito, B.V. Rangan, Development and properties of low-calcium fly ash-
based geopolymer concrete, Res. Rep. GC. 94 (2005). http://www.geopolymer.
org/fichiers_pdf/curtin-flyash-GP-concrete-report.pdf.
[16] A. Hawa, D. Tonnayopas, W. Prachasaree, Performance evaluation and
microstructure characterization of metakaolin-based geopolymer containing
oil palm ash, Sci. World J. 2013 (2013), https://doi.org/10.1155/2013/857586.
[17] M.B. Kahsay, J. Paintin, A. Mustefa, A. Haileselassie, M. Tesfay, B. Gebray,
Theoretical and experimental comparison of box solar cookers with and
without internal reflector, Energy Procedia 57 (2014) 1613–1622, https://doi.
org/10.1016/j.egypro.2014.10.153.
[18] X. Li, Z. Wang, Z. Jiao, Influence of curing on the strength development of
calcium-containing geopolymer mortar, Mater. (Basel). 6 (2013) 5069–5076,
https://doi.org/10.3390/ma6115069.
[19] S. Mahavar, P. Rajawat, R.C. Punia, N. Sengar, P. Dashora, Evaluating the
optimum load range for box-type solar cookers, Renew. Energy 74 (2015) 187–
194, https://doi.org/10.1016/j.renene.2014.08.003.
 M. Zahid et al. / Construction and Building Materials 181 (2018) 227–237
[20] F.A. Memon, M.F. Nuruddin, S. Demie, N. Shafiq, Effect of curing conditions on
the strength of fly ash based self compacting geopolymer concrete, Int. J. Civ.
Environ. Struct. Constr. Archit. Eng. 5 (2011) 8–22.
[21] A. Mustafa Al Bakri, H. Kamarudin, M. Bnhussain, A.R. Rafiza, Y. Zarina, Effect of
Na2SiO3/NaOH ratios and NaOH molarities on compressive strength of fly-
ash-based geopolymer, ACI Mater. J. 109 (2012) 503–508.
[22] A. Mustafa Al Bakri, H. Kamarudin, M. Hussain, I.K. Nizar, Y. Zarina, A.R. Rafiza,
The effect of curing temperature on physical and chemical properties of
geopolymers, Phys. Procedia 22 (2011) 286–291, https://doi.org/10.1016/j.
phpro.2011.11.045.
[23] T.R. Naik, F. Asce, Sustainability of concrete construction, Pract. Period. Struct.
Des. Constr. (2008) 98–103.
[24] S.S. Nandwani, Solar cookers—cheap technology with high ecological
benefits, Ecol. Econ. 17 (1996) 73–81, https://doi.org/10.1016/0921-8009
(96)00021-3.
[25] S.K. Nath, S. Kumar, Influence of iron making slags on strength and
microstructure of fly ash geopolymer, Constr. Build. Mater. 38 (2013) 924–
930, https://doi.org/10.1016/j.conbuildmat.2012.09.070.
237
[26] F.N. Okoye, J. Durgaprasad, N.B. Singh, Fly ash/Kaolin based geopolymer green
concretes and their mechanical properties, Data Br. 5 (2015) 739–744, https://
doi.org/10.1016/j.dib.2015.10.029.
[27] Sindhunata, J.S.J. Van Deventer, G.C. Lukey, H. Xu, Effect of curing temperature
and silicate concentration on fly-ash-based geopolymerization, Ind. Eng.
Chem. Res. 45 (2006) 3559–3568, https://doi.org/10.1021/ie051251p.
[28] B.V.R.M.D.J. Sumajouw, Low-calcium fly ash-based geopolymer concrete :
reinforced beams and columns, Concrete (2006) 1–120.
[29] K. Vijai, R. Kumutha, B.G. Vishnuram, Effect of types of curing on the strength
of geopolymer concrete, Int. J. Phys. Sci. 5 (2010) 1419–1423. http://www.
academicjournals.org/IJPS.
[30] D. Zaharaki, K. Komnitsas, V. Perdikatsis, Use of analytical techniques for
identification of inorganic polymer gel composition, J. Mater. Sci. 45 (2010)
2715–2724, https://doi.org/10.1007/s10853-010-4257-2.
[31] M. Zahid, N. Shafiq, M.F. Nuruddin, E. Nikbakht, A. Jalal, Effect of partial
replacement of fly ash by metakaolin on strength development of fly ash based
geopolymer mortar, in: Key Eng. Mater., Trans Tech Publications, Switzerland,
2017, pp. 131–135, https://doi.org/10.4028/www.scientific.net/KEM.744.131.