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Utilization of high volume cement kiln dust and rice husk ash in the
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DOI: 10.1016/j.jclepro.2019.05.056

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 Journal of Cleaner Production 230 (2019) 592e602

Contents lists available at ScienceDirect

Journal of Cleaner Production

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

Utilization of high volume cement kiln dust and rice husk ash in the
production of sustainable geopolymer
Sajad Yaseri a, Vajihollah Masoomi Verki a, Mahdi Mahdikhani b, *
a
Department of Civil Engineering, Qazvin Branch, Islamic Azad University, Qazvin, Iran
b
Department of Civil Engineering, Imam Khomeini International University, Qazvin, Iran

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

Article history: This study investigates the feasibility of using combination of Cement Kiln Dust (CKD) which is classified
Received 30 September 2018 as a hazardous solid waste material and Silica Fume (SF), as a sustainable precursor to make binary
Received in revised form binder based geopolymer paste. Furthermore, Rice Husk Ash (RHA) an agricultural waste is used as the
4 May 2019
main source for preparing amorphous silica in order to produce sustainable sodium silicate solution and
Accepted 5 May 2019
Available online 9 May 2019
also to replace it with the standard commercial sodium silicate. In this study alkaline activator solution
was prepared through the combination of RHA powder with 10-M sodium hydroxide solution (NaOH) to
adjust the Na2O/SiO2 and H2O/Na2O molar ratio. Geopolymer paste was produced by mixing different SF/
Keywords:
Geopolymer
CKD proportion (15/85%, 30/70%, 45/55%, 50/50%, 55/45%, 70/30% and 85/15% by weight) with the RHA-
Microstructure NaOH alkaline activator solution. The compressive strength test, Fourier transform infrared spectroscopy
Sustainable activator solution (FTIR), mini-slump test, setting time and X-ray diffraction (XRD) were carried out to characterize the
Cement kiln dust geopolymer. The results show that it was feasible to make sustainable geopolymer with combination of
Alternative cement SF/CKD binder and sodium silicate solution from RHA. By increasing CKD up to the optimum amount
Green material (45%) the compressive strength increased linearly and then the compressive strength decreased when it
exceeds the optimum amount. The results also showed that the setting time of the geopolymer can be
modified by changing the SF/CKD proportion. Moreover, the XRD presented that the geopolymer paste
has an amorphous to semi-crystalline phase. Also, FTIR analysis illustrated that by increasing silica
content, Si-O-Si (Al) bonds which are considered as the geopolymeric fingerprint area, will shift to the
higher wavenumber.
© 2019 Elsevier Ltd. All rights reserved.

1. Introduction
The Portland cement is widely used in construction industry;
however, it has destructive environmental impacts; because its
production needs a lot of energy and it emits large quantities of
carbon dioxide and thus it contributes in making the earth warmer
(Chindaprasirt and Chalee, 2014; Sun et al., 2013). For example, in
order to produce 1 ton of OPC, 1.7 tons of raw materials are
consumed and 0.8 tons of CO2 are entered into the atmosphere
(Huntzinger and Eatmon, 2009).
Today, to achieve a sustainable construction industry, the
alternative cements have been extensively investigated (Scrivener
et al., 2018). Geopolymer is a kind of material which is obtained
* Corresponding author.
E-mail addresses: s.yaseri@qiau.ac.ir (S. Yaseri), vmv.masoomi@qiau.ac.ir
(V. Masoomi Verki), mahdikhani@eng.ikiu.ac.ir (M. Mahdikhani).
from the alkaline activator and it can be produced from the in-
dustrial wastes or by-products (Duxson et al., 2007; Van Deventer
et al., 2012). One of the key advantages of geopolymer is the
reduction of 40%e80% in the emission of greenhouse gases,
compared with OPC (Habert et al., 2011; McLellan et al., 2011). Also,
its other advantage is that it has the capability of reusing industrial
by-products or the other wastes as the major component of the
geopolymer binders.
Cement Kiln Dust (CKD) is a dangerous by-product, which is
produced in large quantities when Portland cement is made
(Maslehuddin et al., 2008). It is estimated that the production of
CKD is about 15%e20% to that of Clinker (Kunal et al., 2012).
Million tons of CKD are annually produced worldwide and most of
it is buried as waste matter and rubbish. Not only does the
disposal of CKD take up a lot of land, but also it contaminates the
ground waters (Kunal et al., 2014). CKD increases the cost of
cement factories due to the loss of materials and also using the
energy for collecting, reprocessing and land filling (Khater and

https://doi.org/10.1016/j.jclepro.2019.05.056
0959-6526/© 2019 Elsevier Ltd. All rights reserved.
 S. Yaseri et al. / Journal of Cleaner Production 230 (2019) 592e602 593

Zedane, 2012). Reusing this product significantly reduces the they introduced the replacement of 75% of RHA-NaOH solution
waste inside the factory and it also reduces the need for raw instead of the industrial sodium silicate as a suitable solution for
materials; this can help us to preserve natural resources. Today, producing the sustainable geopolymer and reducing the global
significant advances have been made in managing and reusing the warming.
Cement Kiln Dust (Salem and Salem, 2017). Typically, CKD is an The purpose of this study is to determine the feasibility of
alkaline substance and this feature is one of the main reasons for making binary binder geopolymer paste including sodium silicate
its removal from cement. Generally, the pH of a CKD water solution from RHA, CKD and SF powder with different percentages
mixture was reported more than 12 (Kunal et al., 2014, 2012); and of substitution such as 15, 30, 45, 50, 55, 70, and 85 percentages and
due to high alkalinity, it is mainly not returned to cement pro- with constant binder to solution ratio (B/S) of 1.4. Also, in this study,
duction cycle (Salem et al., 2012). Corish and Coleman. (1995) an alkaline activator solution was made of the combination of the
have reported that alkalinity of CKD depends on the particle size amorphous Rice Husk Ash with 10 M NaOH, and the industrial so-
in a way that the smaller CKDs have more alkalinity. XRD analysis dium silicate solution (waterglass) was completely removed, in
showed that CaCO3, SiO2, and CaSO4 are the main components of order to produce a sustainable geopolymer and also in order to
CKD (Salem et al., 2015). Maslehuddin et al. (Maslehuddin et al., have a significant economic benefits. Geopolymer paste was made
2008) has studied the impact of replacing Portland Cement (PC) from mixing the binary-binder powder with RHA-NaOH activator
with CKD on setting time; they replaced 0, 5% and 10% of the solution with constant Molar ratio of H2O/Na2O and Na2O/SiO2 in
weight of the paste with CKD. With increasing the replacement of an alkaline activator solution. The relationship between the influ-
CKD instead of PC, the water demand increased and the setting ence of SF/CKD proportion on the compressive strength in different
time decreased. On the one hand, using CKD increases alkalinity in ages of 1, 7 and 28 was studied. Furthermore, the relationship be-
the alkaline activator solution, thus it can reduce the demand for tween the influence of the SF/CKD proportion and Ca/Si molar ratio
NaOH and make the production of geopolymer cost-effective on the setting time, workability and T20 (flow time of the fresh
(Ahmari and Zhang, 2013). paste) was analyzed. The characteristics of the paste were identified
An alkaline solution is prepared mainly from a compound or a by FTIR and XRD analysis. The Molar ratios of geopolymer paste
mixture of alkaline hydroxide such as NaOH or KOH with in- (Na2O/CaO, CaO/SiO2, SiO2/Al2O3, Na2O/SiO2, H2O/Na2O, Na/Si, Na/
dustrial sodium silicate or potassium silicate. These industrial Ca, Ca/Si, Si/Al, water/Solid, water/binder and Na2O/Binder) in each
silicates solution are used in order to provide a soluble silicate in mixture were calculated.
an alkaline solution; however, these industrial silicate have the
highest contribution in the environmental effects and they are
2. Material and methods
the most expensive constituents in the production of geopolymer
(Habert et al., 2011). Habert et al. (2011) showed that using the
2.1. Materials
industrial sodium silicate (waterglass) will increase the envi-
ronmental pollution by about 1000%, such as freshwater eco-
In this paper, Cement Kiln Dust (CKD) and Silica Fume (SF) were
toxicity.
used as precursor. Also, RHA-NaOH solution was used as an alter-
One of the methods of supplying soluble silicates and
native to the commercial sodium silicate. CKD was received as dry
reducing these industrial silicates is using the industrial waste
powder from Abyek Cement Factory in Qazvin, Iran. The loss on
and side products such as waste glass and Rice Husk Ash (RHA).
ignition (LOI) of CKD at 900
C is 33.6%, it is attributed to carbon-
Agro-industrial waste such as RHA has a good potential for the
ation and water. The Rice Husk (RH) was prepared from a rice mill
usage as an amorphous silicate source in an alkaline activator
in Alamut region of Qazvin, Iran. The RHA was obtained by burning
solution (Bouzo  n et al., 2014); because it is economical and also it
the Rice Husk at 650
C for 6 h. Table 1 presented the chemical
easily dissolves in a high density hydroxide solution. Among
composition of CKD, RHA, and SF powder which obtained from X-
various types of by-products, which have a lot of recyclable and
ray fluorescence (XRF) analysis. Fig. 1 show the XRD pattern of RHA,
reusable energy resources, Rice Husk (RH) is a potential source of
CKD and SF respectively. Particle size distribution curves of RHA,
energy (Li et al., 2011; Vlaev et al., 2003). The annual production
CKD and SF have been shown in Table 2 and Fig. 2, respectively.
of Rice Husk around the world is about 70e80 million tons
NaOH powder in the flakes form with the purity of 98% was used.
(Kizhakkumodom Venkatanarayanan and Rangaraju, 2015; Lu
et al., 2008) which is traditionally buried as waste (Kamath and
Proctor, 1998; Li et al., 2011). But, this can lead to the creation 2.2. Preparation of RHA-NaOH activator solution and binary binder
of a pollution source and a decrease in water quality and, based geopolymer paste
consequently a kind of disruption in the environment (Rodríguez
de Sensale, 2006). The Rice Husk is combustible and due to the The RHA-NaOH sodium silicate solution was prepared by mixing
high thermal value or calorific power (approximately 16720 kJ/ RHA powder and 10-Molar NaOH solution. To prepare the alkaline
kg), it is used as fuel in boilers and power generators solution, NaOH powder was first mixed with water, and then
(Suksiripattanapong et al., 2017), and the remainder of this
combustion process is the Rice Husk Ash (RHA). Table 1
Chemical composition of raw materials (XRF Analysis).
The release of the RHA into ecosystem has had many criticisms
and complaints, mostly because of the carcinogenicity of RHA (Foo Composition SF (%) CKD (%) RHA (%)
and Hameed, 2009). Due to the high pozzolanic activity of the CaO 0.75 45 1.2
existing silica in RHA (90e95%), it can be replaced by Waterglass as SiO2 85.19 11 88
a soluble silicate source in the alkaline solution to help us have a Al2O3 0.3 3 0.1
Fe2O3 3.41 2.7 0.58
clean environment. The studies by Cherdsak Suksiripattanapong
MgO 2.1 2.11 0.99
(Suksiripattanapong et al., 2017) showed that alkaline activator K2O 2.17 1 2.2
solution made of RHA, has similar manner and results compared to Na2O 1.5 0.2 0.1
a traditional alkaline activator solution and it sometimes has had TiO2 0.05 0.18 0.03
better effects. Kamseu et al. (2017) studied the replacement of the LOI* 3.8 33.9 5

combination of RHA and NaOH instead of industrial sodium silicate; *Loss on Ignition (900
C, 1 h).
594 S. Yaseri et al. / Journal of Cleaner Production 230 (2019) 592e602
Fig. 1. XRD pattern of RHA, CKD and SF.
Table 2
d10, d50 and d90values of the CKD, SF and RHA.
sample d10(mm) d50(mm)
CKD 0.67 2.55
SF 0.11 3.12
RHA 9.10 42.74
suitable amount of RHA was added to NaOH solution. In order to
have a homogenous solution, the mixture was well mixed for
40 min, and then it is allowed to be cooled at the room temperature
and then it was saved for 24 h before using (Kamseu et al., 2017).
RHA-NaOH activating solution was prepared with H2O/Na2O and
Na2O/SiO2 molar ratio equal to 11.5 and 1.0. CKD and SF became
homogenous by using the mechanical mixer (ASTM C305, 2014).
Then, RHA-NaOH activator solution was added gradually and in
order to have homogeneous slurry it was mixed for 10 min by using
a mechanical mixer. CKD powder was replaced with SF with the
percentages of 15, 30, 45, 50, 55, 70, and 85. In all of the samples,
the powder and the RHA-NaOH activator solution were mixed with
a B/S constant ratio equal to 1.4. The details of the mixtures have
been listed in Table 3. According to ASTM C109/C109M0 (ASTM
C109, 2016) fresh paste was poured in 50-mm cube Plexiglas
molds. Then, all Specimens were vibrated in order to eliminate the
entrapped air. According to a recent study (Yaseri et al., 2017) the
specimens were covered with a polythene sheet to prevent the
reduction of moisture. The specimens were placed inside an oven at
60
C for 24 h to be cured at this temperature. The samples were
taken out of the molds and they were placed inside a plastic bag in
order to prevent cracks at room temperature.
Fig. 2. Particle size distribution of CKD, SF and RHA.
2.3. Characterization techniques
2.3.1. Setting time
In order to evaluate the setting time of geopolymer paste the
ASTM C191 standard test method (ASTM C191, 2013) was used. The
penetration of Vicat Needle was measured according to previous
study (Yaseri et al., 2017). The penetration time of 25 mm is known
as its initial setting time. The time at which geopolymer paste be-
comes stiff and the needle cannot penetrate into the paste is final
setting.
d90(mm) 2.3.2. Mini slump test
9.16 Mini slump test was used to evaluate the flowability of the fresh
19.89 paste based on EFNARC (EFNARC, 2002). T20 slump flow test was
74.07 also performed to evaluate the flowability of the fresh paste. The
mini slump was placed at a glassy graduated plate (Fig. 3) and it was
filled with the fresh geopolymer paste, afterwards immediately the
cone was removed vertically and the paste flowed. When the flow
of the paste stopped, the average of the two perpendicular di-
ameters was measured as the mini slump spread. Also, T20 has been
defined as the needed time for removing the mini slump until the
paste reaches a circle with diameter of 20 cm. In this study, T20 was
registered by a camera which was set up directly above the mini
slump and the graduated plate. Fig. 4 shows the details of the po-
sition of the digital camera at the top of graduated plate. At the
recent studies (Yaseri et al., 2018), this method was used to record
more accurate laboratory data and to eliminate the human errors.
2.3.3. Compressive strength
Compressive strengths tests of all Geopolymer samples were
measured according to ASTM C109 (ASTM C109, 2016). At the end of
curing period all samples were removed from oven. They then were
put at ambient temperature until the day of testing. The specimens
were tested at the ages of 1, 7 and 28. For each ratio three specimen
were tested.
2.3.4. X-ray diffraction (XRD)
XRD- Philips PW1730 X-ray diffractometer with Cu Anode Ma-
terial and scanned from 10
to 80

2 Th at 0.05
2Th.steps, was
 S. Yaseri et al. / Journal of Cleaner Production 230 (2019) 592e602 595

Table 3
Detail of mixture proportions.

COMPOSITION OF GEOPOLYMER

SOLUTION PASTE

Concentration Molar ratio Mass ratio Molar ratio

of NaOH
mix code SiO2/ H2O/ SF CKD Binder/ Water/ Water/ Na2O/ SF/ CaO/ SiO2/ Na2O/ Na2O/ Ca/ Si/ Na/ Na/
Na2O Na2O % % Solution Solid Binder Binder % CKD ratio SiO2 Al2O3 SiO2 CaO Si Al Si Ca

15SF-85CKD 10 M 1.0 11.5 15 85 1.4 0.41 0.31 13.0 0.17 1.16 23.0 0.35 0.30 1.77 20.4 0.57 0.32
30SF-70CKD 10 M 1.0 11.5 30 70 1.4 0.41 0.31 13.0 0.42 0.73 36.0 0.27 0.37 1.11 31.7 0.43 0.38
45SF-55CKD 10 M 1.0 11.5 45 55 1.4 0.41 0.31 13.0 0.81 0.46 54.5 0.22 0.47 0.71 48.1 0.35 0.49
50SF-50CKD 10 M 1.0 11.5 50 50 1.4 0.41 0.31 13.0 1.00 0.40 62.8 0.20 0.52 0.61 55.5 0.32 0.54
55SF-45CKD 10 M 1.0 11.5 55 45 1.4 0.41 0.31 13.0 1.22 0.34 72.5 0.19 0.57 0.52 64.0 0.31 0.60
70SF-30CKD 10 M 1.0 11.5 70 30 1.4 0.41 0.31 13.0 2.33 0.20 115.5 0.17 0.85 0.30 102.0 0.26 0.88
85SF-15CKD 10 M 1.0 11.5 85 15 1.4 0.41 0.31 13.0 5.66 0.09 207.3 0.14 1.60 0.14 183.1 0.23 1.66

Fig. 3. Mini slump cone and glassy graduated plate.

used to determine the amorphous and crystalline phase of geo-

polymer paste. Given this purpose, the sample was prepared for the
XRD test in the form of a powder dispersed from the No.325 sieve.

2.3.5. Fourier transform infrared spectroscopy (FTIR)

The chemical bonds and molecular vibrations of the samples
were evaluated by The JASCO, FT/IR-6300 (wavelength 4000 cm-1
to 400 cm-1), Japan.
3. Result and discussion
3.1. Workability of geopolymer paste
The results of mini slump spread and T20 with different SF/CKD
proportion have been reported in Fig. 5 and Fig. 6 respectively. The
results of the mini slump showed that the spread of the fresh paste
depends on the SF/CKD proportion. The mini slump spread of all
samples differs from 188 mm to 295 mm. Most spread in 85SF-
15CKD mixture has been observed. Also, the spread of the geo-
polymer paste was the least one in 15SF-85CKD mixture. As shown
Fig. 4. The sketch of the digital camera position at the top of mini-slump test.
in Fig. 5, with an increase in the amount of SF (decrease in CKD), the
mini slump spread increases.
Particle size distribution of binder plays an important role on
spreading fresh paste. Fig. 2 demonstrated that the average par-
ticle size of CKD is smaller than that of SF; therefore, CKD particles
have a more specific surface compared with that of SF. As a result,
when the amount of SF increases, the water demand decreases in
the mixture and it results in an increase in workability. Reducing
the particle size of the binder results in the reduction of the
workability in mortar or concrete (Collins and Sanjayan, 1999).
Also, the study of Maslehuddin et al. (2008) indicated that with an
596 S. Yaseri et al. / Journal of Cleaner Production 230 (2019) 592e602
Fig. 5. Effect of various SF/CKD proportion on mini-slump spread.
Fig. 6. Effect of various SF/CKD proportion on T20.
increase in the replacement of CKD instead of PC, the water de-
mand increases and the workability decreases. Fig. 7 shows the
spread of each mixture.
As shown in Fig. 6, with an increase of SF up to 50%, the flow
time of geopolymer paste (T20) decreased. The reason for this
decrease of the T20 is the larger size of SF particle compared with
those of CKD. On the other hand, as SF increases more, the
decreasing trend is changed and T20 increases. The T20 in the mini
slump test is strongly affected by the viscosity and yield stress (Gao
and Fourie, 2015). An increase in the amount of SF in the binder
leads to an increase in the yield stress in the system and thus it
increases the flow time in the mini slump (Koutný et al., 2018). This
can justify an increase of T20 in the high amount of SF.
In Figs. 5 and 6, the mini slump spread and T20 of mix 15SF-
85CKD and 30SF-70CKD have been shown. Its spread is 188 mm
and in this situation no T20 was recorded. While with an increase in
the amount of SF, the spread in mix 30SF-70CKD became 215 mm
and T20 became 9.8 s. Also, with an increase in the amount of SF for
mix 50SF-50CKD up to mix 85SF-15CKD, the spread and the flow
time of the mini slump increased up to 9.4% and 50%, respectively.
3.2. Setting time
Fig. 8 shows the effects of SF/CKD proportion on the initial
setting time and final setting time of geopolymer slurries at 60
C.
As observed, the Initial setting time varies from 40 to 56 min and
the final setting time were recorded from 45 to 70 min. As shown in
Fig. 8, the geopolymer setting time is strongly correlated with the
amount of CKD and the ratio of Ca/Si. An increase in the amount of
CKD and Ca/Si molar ratio will improve the setting time and it has a
very positive effect on its decrease. With an increase in CKD from
15% to 85%, its initial setting time decreased about 28% and the final
setting time decreased 35%. The reason is that with an increase in
CKD, the amount of calcium hydroxide (Ca(OH)2) increases and the
amount of Caþ2 will increase. As a result, it accelerates the geo-
polymerization reaction. Calcium hydroxide acts as an accelerator
in the activator for hydration reaction and it leads to the production
of more hydration products, thus, it shortens the setting time
(Abdel-Gawwad and Abo-El-Enein, 2016). Also, with an increase in
the amount of CKD, the amount of the dissolved Ca increases and it
leads to an increase in the alkalinity of the system. With an increase
in the alkalinity of the system, more amounts of Si and Al dissolve
and the reaction of geopolymerization accelerates, resulting in an
increase in the setting time. In addition, Ca dissolves in the alkaline
solution sooner than Si and then Ca(OH)2 and CaCO3 yieldes. In XRD
analysis, it was confirmed that by increasing the amount of CKD,
the crystalline phases associated with CaCO3 will increase (Ahmari
and Zhang, 2013). Also, with regard to the particle size distribution
analysis (Fig. 2), CKD particles are smaller than SF and they absorb
more water; consequently, it leads to a faster dehydration and it
decreases the setting time.
The longest setting time was recorded for mix 85SF-15CKD. The
results of the setting time indicated that by increasing SF the setting
time will increase linearly. The reason is that the silica particles
react with each other and form the oligomeric silicates, and the
condensation between these oligomeric silicates creates a rigid 3D
network. By increasing amount of Si in the system, the condensa-
tion process between oligomeric silicates is slow which results in
an increase in the initial and final setting time (Silva et al., 2007;
Yaseri et al., 2017).
The geopolymer's setting time is related to its workability and it
shows how much it will remain in a plastic conditions (Siyal et al.,
2016). Depending on the application and use, the setting time af-
fects the geopolymer mix design parameters. Retardation in the
setting time is definitely important for transportation in far dis-
tances, placing, compaction, storage and processing. On the other
hand, decreasing the setting time and accelerating it is required for
quick repairs of the damaged surfaces (Perna  and Hanzlí
cek, 2016).
In general, the results of the setting time showed that the modifi-
cation of SF/CKD proportion plays an essential role in changing the
setting time and it can be changed depending on the design re-
quirements. The setting time will be decreased by increasing CKD,
and it is increased with an increase in SF.
3.3. Compressive strength
Fig. 9 shows the compressive strength of geopolymer pastes
with various SF/CKD proportion up to 27 days. These results
showed that it was feasible to utilize combination of SF and CKD as
a precursor for make a geopolymer paste with high compressive
strength. Also, the results confirmed that the alkaline activator
solution made from RHA-NaOH has a great potential for dissolving
the particles and the initiating the geopolymerization reaction.
The minimum compressive strength for mix 15Sf-85CKD was
with the amount of 22 MPa and the maximum compressive
strength and optimum amount was seen in mix 55SF-45CKD with
 S. Yaseri et al. / Journal of Cleaner Production 230 (2019) 592e602
Fig. 7. Mini-slump spread for all mixtures.
Fig. 8. Initial and final Setting times of geopolymer pastes at various SF/CKD
proportion.
the compressive strength of approximately 37 MPa. With an in-
crease in the age of the samples, no changes in the compressive
strength were observed; in fact, as expected, during the first 24 h,
the geopolymer paste reached its final strength (Yaseri et al., 2017);
because at high temperatures (in this study 60
C), the degree of
polymerization is accelerated, resulting in the acceleration of
hardening behavior and also in the reduction of setting time at the
early ages (Rovnaník, 2010, Yaseri et al., 2017).
With an increase of CKD from 15% (mix 85SF-15CKD) up to 45%
(mix 55SF-45CKD), the compressive strength increased about 48%.
The reason for increasing the compressive strength by increasing
the CKD to the optimum amount can be expressed in this way:
with an increase in CKD, the dissolved Ca increases, then the
597
Fig. 9. Effect of different SF/CKD proportion and curing age on compressive strengths
of geopolymer paste.
dissolution of these particles increases the alkalinity of the system
and thus it dissolves more Si and Al ingredients and this acceler-
ates the geopolymerization reaction. Also, Ca2þ acts as a charge-
balancing agent for Al in the geopolymer structure during the
geopolymerization process (Ahmari and Zhang, 2013; Khater,
2013). When CKD increase up to the optimum amount, more
particles of Al (alumina species) involve into the reaction and they
participate more in making geopolymeric gel. FTIR analysis clearly
confirms an increase in Al's participation in the main band of Si-O-
Al (section 3.5). Furthermore, the dissolved Ca creates Ca(OH)2
and CaCO3 in the system. On the one hand, Ca(OH)2 increases the
alkalinity in the system and on the other hand, CaCO3 fills the
pores and it participates as a cementing agent in increasing the
compressive strength. XRD and FTIR analysis confirmed that
598 S. Yaseri et al. / Journal of Cleaner Production 230 (2019) 592e602

crystalline phases of CaCO3 and the related bands to CaCO3 groups.

Another reason for increasing the compressive strength by
increasing CKD can be the size of CKD particles. Particle size
analysis (Fig. 2) shows that CKD has very small particles, and this
small size of CKD particles can make them fill the pores and thus
increases the compressive strength. The similar results have been
reported by other authors (Ahmari and Zhang, 2013).
With an increase in the CKD more than the optimum amount
(45%), the compressive strength decreased. The reason is that an
increase in the CKD causes excessive alkalinity in the system, and
also the amount of the dissolved Ca increases in the system and
this causes the crystalline phases of CaCO3 to increase in the
system. Consequently, it makes some disturbance in the process of
forming a geopolymer gel and also in the formation of Si-O-Si and
Si-O-Al bonds. XRD analysis confirms that by increasing CKD, the
intensity of the crystalline phases of CaCO3 significantly increased.
FTIR analysis also showed that the main bands linked to carbonate
(1426 cm-1 and 875 cm-1) will be intensified with an increase in
CKD. In addition, the result of the setting time indicated that by
increasing the CKD more than the optimum amount, the initial
and final setting time sharply decreased. It may be concluded that
fast setting time causes geopolymer bonds to be formed incom-
pletely in the geopolymer gel before being transferred into a ho-
mogeneous structure (Rahim et al., 2014). Consequently, the
compressive strength decreased in mixes 30SF-70CKD and 15SF-
85CKD.
On the other hand, the results of the compressive strength show
that Si content has an important effect on obtaining the compres-
sive strength. By increasing silica fume (increasing amount of Si)
from 15% (mix 15SF-85CKD) up to 55% (mix 55Sf-45CKD), the
compressive strength increases about 60%. The previous reports
have shown that with an increase Si in the system, the compressive
strength also increases (Ozer and Soyer-Uzun, 2015). In this study,
the increase of SiO2 has been done by replacing the various per-
centages of SF with CKD in the raw material powder and also by
using Rice Husk Ash in the alkaline solution. According to XRD
results (Fig. 10), with an increase SF/CKD proportion, the intensity
of crystalline phases of calcite in the structure decreased. As a
result, by decreasing the crystalline phases, the compressive
strength noticeably increased. The reason is that in the mechanism
of the formation of geopolymer, the RHA-NaOH solution dissolves
the CKD and Silica Fume particles. Then, the Al and Si ingredients
react together as Si-O-Al and Si-O-Si bonds in the system. The silica
and Aluminum particles form AlðOHÞ4 and oligomeric silicates.
The polymerization reaction, Si content is very important for the
formation and acceleration of oligomerization between Si and Al.
When the amount of SF increases, more Si particles become avail- Fig. 10. XRD pattern of geopolymer samples with various SF/CKD proportion.
able in order to form Silicate Oligomers and then these oligomers
react with AlðOHÞ4 and also with each other; as a result, they
make a strong three-dimensional network, thus increasing the amorphous peak becomes larger in mixes 70SF-30CKD and 85SF-
amount of Si up to the optimum amount and this increases the 15CKD (Fig. 10). In addition, the FTIR analysis also confirmed that an
compressive strength. excessive increase in the amount of Si and a decrease in the
Similar to the results of CKD, with an increase in the SF more participation of Al in mixes 70 SF-30CKD and 85SF-15CKD made the
than the permitted limit in mix 70SF-30CKD and mix 85SF-15CKD, main band shift to the higher wavenumber which probably shows
the compressive strength decreases about 5.4% and 32% compared the formation of Si-O-Si bonds (Fig. 11).
with the optimum amount, respectively. A decrease in the In general, from the results of the compressive strength, it can
compressive strength by increasing SF more than the optimum be deduced that the use of 45% of CKD (which was introduced in the
amount will probably depend on two reasons. First, with the introduction section as a waste and pollutant of the air) is very
excessive increase in the amount of SF, the amount of CKD de- suitable in order to obtain the optimum compressive strength in
creases; as a result, the amount of Al for participation in Si and the the geopolymer system. This amount is noticeable in order to
formation of Si-O-Al bonds in the system greatly decreases. Also, by reduce this environmental pollutant and its consumption in geo-
decreasing the amount of CKD, the amount of alkalinity and solu- polymer which enhances its matrix. In addition, by completely
bility of the particles decreases. Second, the excessive amount of removing the industrial sodium silicate from the alkaline activator
SiO2 creates the unreactive silicate oligomers in the system. The solution and also by using the Rice Husk Ash, it can be said that the
results of XRD analysis confirmed that with an increase in Si, the produced geopolymer is a Green Material.
 S. Yaseri et al. / Journal of Cleaner Production 230 (2019) 592e602
Fig. 11. IR spectra of geopolymer products with various SF/CKD proportion.
3.4. XRD analysis
XRD pattern of cement kiln dust is presented in Fig. 1. The
presence of the sharp peaks in the CKD pattern is because of the
crystalline phases of Quartz (PDF# 00-033-1161), Calcium Car-
bonate (calcite)(PDF# 00-005-0586), Sylvine (PDF#98-012-2832)
and Halite (PDF# 98-011-5713) and based on XRF analysis (Table 1)
is due to the presence of SiO2, CaO, Na2O and K2O in CKD powder.
There is the highest crystalline phase (major phase) with the
highest intensity in CKD which is related to calcite; while there is
the minor phase in quartz, halite and sylvine. Fig. 1 also shows that
the XRD pattern of silica fume (SF) in which no crystalline phase is
599
observed. It shows that it has an amorphous phase with halo at
2q
between 18
and 30
due to presence of amorphous silica.
Fig. 10 shows the XRD pattern of geopolymer paste with
different SF/CKD proportion. In X-ray diffraction, the presence of
peaks represent a crystalline phase. Also the presence of halo peaks
shows the presence of the amorphous phase in the system. XRD
pattern of all samples of geopolymer paste shows that after mixing
the CKD and SF powder with an alkaline activator solution (NaOH-
RHA) and after the geopolymerization reaction the amorphous
broad peaks shifted to the higher angle (20
e40
). This indicates
the formation of an amorphous aluminosilicate gel and it is
commonly referred to as geopolymer gel Character or Fingerprint
Area of geopolymerization (Yaseri et al., 2017).
The results of the geopolymer XRD pattern shows that this
system has two phases: the amorphous phase of geopolymer gel
and the crystalline phase of calcite and quartz which exist in the
raw material of CKD. It is obvious that after CKD dissolved in the
alkaline solution (RHA þ 10 M sodium hydroxide), the sharp peaks
decreased in CKD. With the increase of CKD replacement, the in-
tensity of the peaks related to the crystalline phase of CaCO3
increased; this shows that a portion of the dissolved Ca reacted to
air and yielded CaCO3 (Ahmari and Zhang, 2013). The FTIR analysis
confirmed the presence of carbonate vibration bands from CO2 3
groups.
With the increase of SF replacement, the intensity of the crys-
talline phases significantly decreases and the amorphous broad
peak increases. It is clear that changes in the peak intensity affect
the compressive strength of samples. As it is seen in Fig. 9, the
compressive strength increased with decreasing the crystalline
phases up to optimum amount. When the SF ratio exceeds the
optimum amount of mix 55SF-45CKD, the peak of the amorphous
phase becomes larger and the intensity of the crystalline phases
decreases, which is clearly seen in the mix 70SF-30CKD and mix
85SF-15CKD. In other words, the size of the amorphous broad peaks
in these mixtures is similar to the X-ray pattern of the SF. The
reason is that the alkaline solution dissolves the particles of CKD
and SF, and Si and Al ingredients are prepared as tetrahedral
aluminosilicate units. The dissolved silicate forms the species of
monomers, dimers and larger oligomers by self-polymerizing. As a
consequence condensation occurs between these oligomeric sili-
cates species together or between oligomeric silicates species and
AlðOHÞ4 (Wang et al., 2005). When the amount of SF powder in
the system increases, the amount of alumina decreases; but the
amount of the soluble silicate increases. With an exceeding increase
in the amount of silicate, more silicate oligomers react with each
other; as a result, the increase in the amorphous peaks in mixes
70SF-30CKD and 85SF-15CKD can be attributed to the polymeri-
zation of the excess silicate oligomers. By observing the compres-
sive strength in these mixtures (Fig. 9), it is seen that due to the
excessive polymerization of oligomeric silicates in the system and
the increase in the amorphous peak, the compressive strength
decreases. FTIR analysis also confirms that with the excessive in-
crease of Si, the intensity of the related Si-O-Si bonds becomes
more and they tend to shift to the higher wavenumber.
In general, X-ray trace of geopolymer showed that after the
dissolution of powder in the alkaline activator solution, the position
of broad hump are slightly moved to the right which shows that
there are some changes in the raw materials in the geopolymer
reaction and this broad hump is the amorphous gel character in the
system. Also, some of the crystalline phases in paste are related to
undissolved CKD particles, but their intensity is less. XRD analysis
showed that calcium carbonates are the major crystalline phases in
the geopolymer. Also, in high content of SF, an increase in
condensation between the oligomeric silicates causes an increase
in the amorphous hump in the geopolymer paste.
600 S. Yaseri et al. / Journal of Cleaner Production 230 (2019) 592e602
3.5. FTIR analysis
The FTIR analysis of CKD powder has been shown in Fig. 11. Most
of the observed bands are related to the Carbonate vibration from
CO23 ions. The strongest band of this group is located at the
wavenumber of 1426 cm-1 and the sharp peak is located at the
875 cm-1 which is related to asymmetric stretching vibration and
bending vibration is from CO2 3 group, respectively. Also, two weak
bands are at 2872 cm-1 and 2979 cm-1, related to carbonate vibra-
tion. The reason is the presence of calcium carbonate (CaCO3) in
CKD, which is confirmed by the XRD analysis in the previous sec-
tion (section 3.4). Broad bands in the range of 3427 cm-1 are due to
stretching vibrations of the eOH groups. The similar amounts have
been reported by the other authors (Lecomte et al., 2006; Martínez
et al., 2014). The adsorption band in the range of 1030 cm-1 is
related to the asymmetric stretching vibration of Si-O-T bonds from
TO4 (T ¼ Si or Al) (Ahmari and Zhang, 2013; El-Refaey, 2016). The
weak absorption band at 797 cm-1 is related to the symmetric
stretching vibrations of Si-O-Si bonds (Saraya and Aboul-Fetouh,
2012). The absorption band in the range of 712 cm-1 is related to
the symmetric stretching vibrations of Si-O-Al and Si-O-Si bonds.
Also, the absorption band of 471 cm-1 is attributed to the bending
vibration of Si-O groups (Khater, 2013; Salem et al., 2012).
Fig. 11 also shows the IR spectra of the Silica fume. The strongest
adsorption bands were observed in 1108 cm-1, 803 cm-1, and
447 cm-1 which are related to the condensed silicate. The broad
bands with the centrality of 1108 cm-1 are related to the asym-
metric stretching vibrations of Si-O-Si bonds from the tetrahedrons
SiO4. The absorption band in the range of 803 cm-1 is related to the
symmetric stretching vibrations of the Si-O-Si bonds and the band
in the range of 477 cm-1 are related to the bending vibration of O-Si-
O (Mostafa et al., 2001). Also, the weak band in the range of
3439 cm-1 and 1623 cm-1 are related to the stretching vibration and
bending vibration of - OH and H-O-H groups, respectively.
The IR spectra of geopolymer paste is presented in Fig. 11. The
adsorption band in the range of 1014e1042 cm-1 is related to the
asymmetric stretching vibration of Si-O-Al and Si-O-Si bonds from
tetrahedrons TO4 (T ¼ Si or Al). This area is the main area of
Aluminosilicate matrix in the formation of a geopolymer which
shows that the raw materials reacted with an alkaline solution. The
result of which is the reaction of geopolymerization (Sore et al.,
2016; Yaseri et al., 2017). This is the famous region of amorphous
Aluminosilicate gel phase, which is also known as the fingerprint
geopolymerization area. The XRD analysis (Fig. 10) also confirmed
that the appeared amorphous peaks shifted to the right compared
with the raw material which is related to the geopolymerization
reaction.
FTIR results indicate that there is a relationship between the Si/
Al ratio and the position of the bands, in a way that with an increase
of the SF ratio from 15% to the optimal amount of 55%, the main
band position increases from 1014 cm -1e1029 cm -1 which shows
transition into the stronger atomic bonds, it is associated with the
formation of a geopolymer gel. This can be the reason for the in-
crease in the compressive strength with the increase of SF. The
compressive strength results showed that by increasing SF of mix
15SF-85CKD to mix 55SF-45CKD, the compressive strength
increased about 60% (Fig. 9). But with the excessive increase in Si
and a decrease in participation of Al in mixes 70SF-30CKD and
85SF-15CKD, these bands have been transferred to 1038 cm-1 and
1042 cm-1 which can be attributed to the Q3 and Q4 amorphous
silica in the precursor (Sore et al., 2016). XRD analysis (Fig. 10)
confirms that with an increase of SiO2, the broad amorphous peak
clearly created.
From another perspective, with an increase in CKD to the opti-
mum amount, the main band at 1038 cm-1 and 1042 cm-1 shifted to
a lower wavenumber. By increasing the degree of Al replacement
instead of Si, the band shifts to the lower wavenumber. Because the
participation rate of aluminum goes higher and it plays an impor-
tant role in the formation of aluminosilicate gel and it has a positive
impact on the enhancement of geopolymerization reaction. The
results of the compressive strength showed that by increasing CKD
from the amount of 15% to the optimum amount of 45%, the
compressive strength increased linearly. The absorption bands of
the range of 1417e1440 cm-1 and also the bands of the range of
874e880 cm-1 are related to the vibrations of carbonate CO2 3
(Lecomte et al., 2006). It is clearly seen that after the geo-
polymerization reaction, the intensity of these bands decreased.
The weak absorption band related to carbonate in 2979 cm-1 and
2872 cm-1, which appeared in the CKD, after the geopolymerization
reaction almost disappeared. Perhaps, the reason can be related to
Ca participation in the geopolymer structure. The presence of the
bands of carbonate groups is due to the presence of Calcite in CKD,
as well as the dissolved proportion of Ca in the system which reacts
to air and forms the crystalline phase of CaCO3. XRD analysis
confirmed that most of the crystalline phases are related to the
presence of Calcite in the system of geopolymer, and by decreasing
the amount of CKD, the intensity of these crystalline peaks is
decreased (Fig. 10).
In the geopolymer paste, the absorption band with the cen-
trality of 711 cm-1 is related to the symmetrical stretching vibration
of Si-O-Al and Si-O-Si bonds and its intensity decreases and dis-
appears gradually when SF increases. By increasing SiO2 in mixes
70SF- 30CKD and 85Sf 15CKD, the bands in the range of
784e785 cm-1 will appear, which are related to the symmetric
stretching vibration of Si-O-Si bonds; this shows the excessive
amorphous silicate. In XRD analysis, amorphous silicate broad peak
has been confirmed. The broad bands between 3400_3600 cm-1 is
related to the stretching vibration of eOH and the bands in the
range of 1634e1664 cm-1 is due to the bending vibration of the H-
O-H groups. This bands apparently shows the absorption of water
enclosed in the cavities of the specimen or water from the surface
of the geopolymer structure (Khater, 2013; Sore et al., 2016).
In general, the present bands can be divided into three cate-
gories: the vibration in the range of 34600e3400 cm-1 and also in
the range of 1664e1623 cm-1 which are related to e OH groups and
the water structure; the vibration in the range of 1440e1400 and
880e870 which are caused by the vibration of carbonate and in the
range of 1100e450 which are related to the vibration of Si-O (Al)
groups. Table 4 shows the ranges of the frequencies with their
associated bands.
Both results of the XRD and FTIR analysis showed that in this
study, CaCO3 is the major Ca-based geopolymer product. Although
some reports have shown that in the produced geopolymer which
is made by the presence of Ca in its raw materials, CSH gel co-
Table 4
Characteristic FTIR bands of geopolymer products.
Characteristic bands Assigned to
3600-3400 cm-1 -OH(stretching vibrations)
1664-1623 cm-1 -OH(bending vibrations)
1440-1417 cm-1 carbonate vibrations
eCO3 (asymmetric stretching vibrations)
880-873 cm-1 carbonate vibrations
eCO3 (out- of-plane bending vibrations)
2987-2965, 2882-2874 cm-1 carbonate vibrations
CeO vibrations in CO2
1032-1014 cm-1 (main band) Si-O-Al(Si) (asymmetric stretching vibrations)
1107 cm-1 Si-O-Si (asymmetric stretching vibrations)
797-781 cm-1 Si-O-Si (symmetric stretching vibrations)
712 cm-1 Si-O-Al(Si) (symmetric stretching vibrations)
477-454 cm-1 Si-O (bending vibration)
 S. Yaseri et al. / Journal of Cleaner Production 230 (2019) 592e602
existed along with the geopolymer gel as a co-product (Buchwald
et al., 2007; Wang et al., 2004; Yip et al., 2005). However, there
has been no trace of CSH gel in this study based on XRD and FTIR
analysis. Similar results have been reported by other authors
(Ahmari and Zhang, 2013; Lecomte et al., 2006). Perhaps, the
reason is that CSH gel is formed by the presence of Si, Ca and water,
and the trend of this formation is slow and it takes a long time;
when the samples are dry cured at high temperature (in this study
60⁰), dehydration is accelerated and water is exhausted from the
pores quickly and some amount remain inside them which is
confirmed by FTIR analysis in the range of 3600e3400 cm-1 and
1664-1623 cm-1 vibrations related to eOH and HOH groups
(Fig. 11). An increase in the curing temperature and acceleration in
the dehydration conditions make the condition highly desirable for
geopolymerization and geopolymerization occurs more quickly. On
the other hand, these conditions have a devastating effect on the
formation of a CSH gel that slowly builds up and lasts for a long
time. Therefore, the probability of CSH gel formation decreases very
much (Ahmari and Zhang, 2013).
4. Conclusion
In this study, the feasibility of using CKD and SF as the sus-
tainable precursor with the sustainable alkaline activator solution
from RHA to make the geopolymer paste with high compressive
strength was investigated. Based on the findings and results of this
study, the conclusions are as follows:
1) The compressive results showed that adding 45% of CKD in the
mix 55SF-45CKD can lead to 48% increase in compressive
strength compared with the mixture having 15% of CKD; this
amount has been introduced as the optimum amount of CKD.
This is due to increasing in the alkalinity of the system; there-
fore, more Si and Al ingredients will be dissolved; thus, poly-
merization reaction will increase. Also, the presence of Ca
during the geoploymerization process acts as charge-balancing
agent for Al in the geoploymer structure and it will make the
geoploymer network more integrated. Furthermore, more
aluminosilicate source is entered into the system and more Si-O-
Al bonds will be formed in the geopolymerization reaction.
2) With an increase of SF up to 55% (optimum mixture, 55SF-
45CKD), the compressive strength increases; because the pres-
ence of Si leads to the formation and strengthening of Si-O-Si
bonds, but in mixes 85SF-15CKD and 70SF-30CKD, as SF ratio
increases, the compressive strength decreases, which is related
to the excess of Si in the system and the presence of unreactive
silicate oligomers.
3) By increasing the age of geopolymer, no significant change in the
compressive strength was observed. In other words, the geo-
polymer paste reached the high compressive at the first 24 h and
when the age of geopolymer paste were older, the compressive
strength increase was insignificant.
4) By modifying SF/CKD proportion, the setting time and hard-
ening of the geopolymer paste can be changed. By increasing
CKD and Ca/Si molar ratio, the geopolymerization process
accelerated and the setting time decreased, which is important
for quick repairs. Also, by increasing SF, the setting time will be
longer, because condensation process between oligomeric sili-
cates is slow. It is suitable for longer workability and
transportation.
5) By increasing CKD the geopolymer paste became stickier and
the mini slump spread decreased; because CKD particles are
smaller than SF and with its increase, the amount of water de-
mand will increase in the system.
601
6) By increasing the ratio of SF/CKD up to 1 (mix 50SF- 50CKD), the
flow time of geopolymer paste (T20) decreased, and the reason
can be the replacement of the larger SF particles instead of CKD,
which reduces the water demand. However, with an increase in
the ratio of SF/CKD to more than 1, due to increasing viscosity
and yield stress with rising SF in the system, the geopolymer
paste will be stickier and T20 will increase again.
7) XRD analysis displayed that the geopolymer pastes have an
amorphous to semi-crystalline phase whose crystal phases exist
in CKD originally. With an increase SF, the intensity of the
crystalline phases decreases or disappears. At mixes 85SF-
15CKD and 70SF-30CKD, the halo peaks shows the characteris-
tics of amorphous phase which is related to excess silicates and
the formation of unreacted oligomeric silicates in the system.
8) Fourier transform infrared analysis revealed that the main band
at the range of 1014e1042 cm-1 indicates geopolymerization
which is related to Si-O-Si (Al) bonds and with the increase in
the amount of SiO2, the main band shifted to the higher wave-
number. Also, with a decrease in the amount of CKD, the in-
tensity of groups which are related to the carbonate vibration in
the range of 1417e1440 cm-1 decreased noticeably.
9) The results of this study show that it is feasible to make sus-
tainable geopolymer with combination of CKD and SF as powder
and sodium silicate solution from RHA. Moreover, this work
reveals that sodium silicate solution from RHA reduces the
environmental impact and it is a suitable alternative alkaline
solution for synthesize of geopolymer paste.
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