Ceramics International xxx (xxxx) xxx

Contents lists available at ScienceDirect

Ceramics International
journal homepage: www.elsevier.com/locate/ceramint

Effect of curing type on microstructure and compressive strength of

geopolymer mortars
Adil Gultekin *, Kambiz Ramyar
Ege University, Engineering Faculty, Civil Engineering Department, 35030, Bornova, Izmir, Turkey

A R T I C L E I N F O A B S T R A C T

Keywords: In this study, the compressive strength and microstructure of pumice, perlite, burnt clay and fly ash geopolymer
Microwave curing mortars were investigated. Activator solutions with 1.0, 1.2, 1.6 and 2.0 Ms (silica/sodium oxide) ratios as well
Energy saving as 4, 8 and 12% sodium oxide ratios by weight of aluminosilicate material were used. Both oven curing and
Pumice
microwave curing were applied. According to the results, compressive strengths of microwave-cured pumice-,
Perlite
Geopolymer
perlite- and burnt clay-based geopolymer mortars were 5.7, 54.7 and 15.5% higher than those of the oven-cured
counterparts. However, the strength of fly ash geopolymer reduced upon microwave curing. The energy con­
sumption per unit compressive strength in the microwave-cured mortars was found to be between 77.1–87.0%
lower than those of the oven-cured ones, depending on the aluminosilicate type. The changes caused by the
curing type in the microstructure were investigated by SEM/EDS, XRD, FT-IR and thermogravimetric analysis.

1. Introduction materials in geopolymer production will reduce these environmental

Concrete is the most widely used building material in the world [1].
Cement production causes a significant amount of greenhouse gases,
especially carbon dioxide which is released due to the calcination of
limestone and combustion of fossil fuel required to maintain clinkering
high temperature and grinding of either raw materials or clinker [2]. It is
known that approximately one ton of carbon dioxide is emitted during
production of one ton of the portland cement [3]. Moreover, other
hazardous wastes such as mercury be generated during cement pro­
duction and coal burning [4]. Quarrying the limestone required in
cement production causes not only depletion of the natural resources but
also results in both land and water pollution [5]. The search for more
environmentally friendly binder materials alternative to portland
cement has been going on for a long time [6].
Geopolymers have advantages such as low energy consumption,
reduction of carbon dioxide emission and disposal of the industrial
waste products [7]. Duxson et al. [8] revealed that geopolymers can
reduce carbon dioxide emissions by at least 80% compared to that of the
portland cement. Thus, geopolymers attract the attention of more and
more researchers day by day due to their environmental-friendly and
sustainable characteristics [9].
Storage of industrial waste materials such as fly ash, blast furnace
slag, rice husk ash pollutes the environment. The use of such waste
damages [10]. Natural pozzolans have also high potential for geo­
polymer production due to their advantages such as being rich in silica
and alumina as well as relative low mining and transportation costs
[11]. However, there are few studies on the production of alkali acti­
vated binders, especially with natural pozzolans other than metakaolin.
According to Robayo-Salazar and Gutiérrez [12] while there are 7000
articles on alkali-activated materials and geopolymers between 2000
and 2018 years, only 60 articles were found on the natural volcanic
pozzolans. However, even these limited publications show that natural
pozzolans can be successfully used in the geopolymer production.
During the production of geopolymers, electrical energy is generally
required for thermal curing. Suwan et al. [13] stated that for a sufficient
geopolymer strength, 6–48 h curing at 40–90◦ C is required. According to
the International Energy Agency [14], 38% of the electricity produced
worldwide in 2018 was from coal and 10% from nuclear power plants.
Generating energy from coal is one of the most important causes of air
pollution in the world. Combustion of coal causes emission of harmful
particles such as SOx, NOx and volatile organic compounds [15] as well
as high amount of CO2 [16]. There are also certain worries in generating
electricity from nuclear plants. Especially the disasters in Fukushima,
Chernobyl and Three Mile Island increased the doubt about the confi­
dence of nuclear energy. Even the modern nuclear reactors are suscep­
tible to the radioactive leakage caused by possible accidents, sabotage or

* Corresponding author.
E-mail addresses: adilgultekin05@gmail.com (A. Gultekin), kambiz.ramyar@ege.edu.tr (K. Ramyar).

https://doi.org/10.1016/j.ceramint.2022.02.163
Received 7 November 2021; Received in revised form 11 February 2022; Accepted 16 February 2022
Available online 22 February 2022
0272-8842/© 2022 Elsevier Ltd and Techna Group S.r.l. All rights reserved.

Please cite this article as: Adil Gultekin, Kambiz Ramyar, Ceramics International, https://doi.org/10.1016/j.ceramint.2022.02.163
A. Gultekin and K. Ramyar Ceramics International xxx (xxxx) xxx

terrorist attack. In addition, the disposal and storage of nuclear waste Table 1
are still among the biggest problems in nuclear energy [17]. For these Chemical composition and some physical properties of aluminosilicates.
reasons, studies on microwave curing have started in order to produce Chemical composition (%) Pumice Perlite Burnt clay Fly ash
geopolymer with less energy consumption. Graytee et al. [18] stated
SiO2 71.48 73.20 73.65 44.23
that curing temperatures reaching 100◦ C should be used for a long time, Al2O3 13.26 11.65 16.24 19.60
however, curing time above 6 h is unaffordable and impractical for Fe2O3 1.06 1.26 0.79 7.79
production of geopolymer in the traditional oven curing method. SiO2+Al2O3+Fe2O3 85.80 86.11 90.68 71.62
However, it is possible to produce geopolymers that gain strength CaO 0.49 0.84 0.32 4.81
MgO 0.15 0.06 0.16 2.00
rapidly by microwave curing. There are limited studies in the literature Na2O 2.77 2.81 0.07 1.17
on the use of microwave curing in the production of K2O 6.23 4.35 0.19 1.70
geopolymer/alkali-activated materials. Somaratna et al. [19] compared TiO2 <0.01 0.08 0.30 0.44
the effect of oven curing (at 75◦ C for 48 h) and microwave curing (at P2O5 0.01 <0.01 0.28 0.67
SO3 0.79 0.14
240 W for 30, 45, 60, 75, 90 and 120 min) on the properties of alkali <0.01 <0.01
Loss of ignition 4.51 5.10 5.35 17.36
activated fly ash mortars. In spite of short curing time, microwave-cured Physical property
specimens gained similar or higher compressive strength than that of Blaine specific surface (cm2/g) 7634 4946 8680 3506
oven-cured specimens. Greytee et al. [18] determined that Class F fly Specific gravity 2.36 2.26 2.67 2.35
ash-based geopolymer pastes cured in the microwave for 15 min at 200,
300, 400 and 600 W, can reach 59, 72, 67 and 54 MPa compressive
fly ash is majorly arisen from its unburned carbon content. In spite of
strength, respectively. In addition, it was reported that prolonging the
grinding for the same time in the same grinder, the lower fineness of the
curing time to 60 min, increased the compressive strength to around 90
perlite particles (than that of pumice particles, Fig. 1) was attributed to
MPa. El-Feky et al. [20] subjected alkali-activated ground granulated
its higher resistance to the degradation. It is evident that, except for fly
blast furnace slag pastes to microwave curing for 2, 4, 6 min at 720 W. It
ash which consists of spherical particles, the particles of the other alu­
was reported that the 7-day compressive strength of 2 min microwave
minosilicates are majorly angular or irregular in shape. From Fig. 1 the
cured specimens exceeded 50 MPa which increased to 60 MPa at 28 days
median particle size (d50) of pumice, perlite, burnt clay and fly ash were
age. Tan et al. [21] investigated the effect of ambient and microwave
found to be 13.9, 22.9, 13.2, and 25.6 μm respectively.
curing by replacing 0, 10, 25, 40, 55% of ground recycled aggregate
powder with metakaolin and found the efficiency of microwave curing
to increase the compressive strength in spite of low energy consumption. 2.2. Method
Shi et al. [22] investigated the effect of oven and microwave curing,
applied for 4.5 h at the same temperatures, on the compressive strength Activator solutions with 1.0, 1.2, 1.6 and 2.0 Ms ratios (SiO2/Na2O
of alkali-activated fly ash pastes. It was observed that, in spite of ratio by weight) as well as 4, 8 and 12% Na2O contents (Na2O content of
consuming 26.4% less energy, the compressive strength of the samples the activator solution/weight of aluminosilicate) were prepared by
cured in the microwave was 26.9% higher than that of the oven-cured dissolving sodium hydroxide pellets in sodium silicate solution. The
specimens. Several researchers using natural loess [23], high-lime fly solutions were used after resting for 24 h at room temperature. The
ash [13,24] and bottom ash [25] showed that microwave curing could mortar mixtures are designated according to their aluminosilicate ma­
be an alternative curing method in geopolymer production. terial, Ms ratio and Na2O content. For example, Pm 1.0–4 is a mixture
In this study, the microstructure and compressive strength of geo­ containing pumice and an activator with Ms ratio of 1.0 and Na2O
polymer mortars containing Class F fly ash, burnt clay and natural content of 4%.
pozzolans (pumice and perlite) cured in the oven or microwave were While preparing the mixtures, sand, aluminosilicate material, acti­
examined. The changes in microstructure of geopolymers were investi­ vator solution and water, if any, were put into the mixer, and the mixer
gated in detail by SEM/EDS, XRD, FT-IR and thermogravimetric anal­ was operated for 90 s at low speed. After scraping off the mortar adhered
ysis. Moreover, the energy requirement to attain a given strength in the to the mixer, mixing was continued for another 90 s at the same speed.
oven- and microwave-cured mortars was compared. Then the mortars were placed in 50 mm metallic cube molds in two
layers and each layer was compacted by 25 drops from the jolting table.
2. Materials and method Oven-cured samples were placed in the oven with their molds immedi­
ately after preparation. In order to prevent the fresh mortars from
2.1. Materials thermal shock, the oven was operated after placing of the samples. The
rate of increasing temperature was approximately 10◦ C/min and the
Four aluminosilicate materials, i.e., pumice, perlite, burnt clay, and curing time was started after the oven reached the curing temperature.
Class F fly ash were used in the geopolymer mixtures. The pumice and The time and temperatures selected for the oven curing were
perlite were commercial materials with particles in the range of 0–250 60◦ C–72 h, 90◦ C-48 h and 120◦ C-24 h. At the end of the curing period,
μm which were further reduced by grinding in a laboratory type plan­ the mortars were removed from the oven, and demolded after cooling to
etary ball mill (at 500 rpm for 5 min). Burnt clay was prepared in the the room temperature. The compressive strengths of specimens were
laboratory by burning kaolin at 600◦ C for 1 h. No grinding was neces­ determined with a 2000 kN hydraulic testing machine at a loading rate
sary after burning of the clay. The chemical composition/some physical of 0.9 kN/s.
properties, particle size distributions and SEM views of aluminosilicate The microwave-cured specimens were prepared in the same way as
materials are shown in Table 1, Figs. 1 and 2, respectively. A sodium the oven-cured ones. However, these specimens were covered with high
silicate solution consisting of 23.2% SiO2, 10.0% Na2O and 66.8% H2O, temperature resistant moisture proof bags as shown in Fig. 3 and kept in
by weight, and a granular sodium hydroxide with 98% purity were used the oven at 60 or 120◦ C (60◦ C for fly ash, 120◦ C for pumice, perlite and
as alkali activators. The sand used in the preparation of the mortar mixes burnt clay) for various times (3 h for burnt clay, 4 h for pumice and
was standard CEN sand. Tap water was added to adjust the consistency perlite, 5.5 h for fly ash) until they could be demolded safely. These
of the mixtures (if any). periods were sufficient for the mixtures to gain required rigidity for
As it can be seen from Table 1, the SiO2+Al2O3+Fe2O3 contents of demolding without considerable strength gain. The samples taken out of
pumice, perlite and burnt clay are far above 70% while their CaO con­ the oven were demolded after cooling to room temperature and sub­
tents are below 1%. The corresponding values are 71.62% and 4.81%, jected to microwave curing at 450, 600 and 800 W for 5, 10 and 15 min.
respectively, for the fly ash. Moreover, the 17.36% loss on ignition of the A household microwave oven with a maximum capacity of 800 W was

2
A. Gultekin and K. Ramyar Ceramics International xxx (xxxx) xxx

Fig. 1. Particle size distribution of aluminosilicates.

Fig. 2. SEM views of aluminosilicates.

Fig. 3. Microwave cured fly ash geopolymer a) before oven precuring, b) after 5.5 h oven precuring, c) after microwave curing at 450 W for 15 min.

3
A. Gultekin and K. Ramyar Ceramics International xxx (xxxx) xxx

used for curing.
2.3. Mixtures
The mix proportions, flow diameters and fresh unit weights of the
mortars are shown in Table 2. The flow diameter (determined according
to TS EN 459-2 [26]) of the mortars were kept constant as 155 ± 5 mm.
However, due to the considerable differences between the morphology,
surface texture and fineness of the aluminosilicates, water requirement
of the mixtures for the target flow was quite different. Moreover, in some
of the mixtures having high activator content, the flow exceeded the
target value even without any water addition.
3. Results and discussion
3.1. Oven curing
The compressive strengths of geopolymer mortars are presented in
Figs. 4–6. The compressive strengths of pumice, perlite and burnt clay
mortars were very low at 60◦ C-72 h curing regime. Taxiarchou et al.
[27] stated that after curing at 70◦ C for 48 h, the perlite geopolymer
specimens were still in the plastic state, so that their compressive
strength could not be determined. It was concluded that, perlite-based
geopolymers require more curing time than the other materials. In
Taxiarchou et al. study 50 mm perlite geopolymer showed about 30 MPa
compressive strength when cured at 70◦ C for 5 days. Kurt [28], in a
similar study, stated that 40 mm cube pumice geopolymer mortars,
cured at 60◦ C for 7 days, gained 45.5 MPa compressive strength. In the
present study, the curing temperature of 60◦ C was found to be insuffi­
cient for the strength development in the pumice, perlite and burnt clay
mixtures. The fact was probably arisen from the deficiency of the tem­
perature to help release the Al and Si species from these
aluminosilicates.
Considerable improvement in the compressive strengths of perlite-,
pumice- and burnt clay-based geopolymers was observed as the curing
temperature increased to 90 or 120◦ C. The most favorable curing tem­
perature and time for these geopolymers were found to be 120◦ C and 24
h. The compressive strength of the burnt clay-based geopolymer mortars

Table 2
Mix proportions, flow diameter and unit weights of mortars.
Asa Na2O (%) Mixture Materials (g) Property

As Sand Activator solution Water Flow diameter (mm) Unit weight (kg/m3)

Ms: 1.0 Pumice 4 Pm 1.0–4 450 1215 91.4 185.5 150 2131.5
8 Pm 1.0–8 182.8 137.5 151 2177.6
12 Pm 1.0–12 274.2 80.5 152 2194.7
Perlite 4 Pr 1.0–4 91.4 156 153 2175.2
8 Pr 1.0–8 182.8 100 151 2208.3
12 Pr 1.0–12 274.2 61 155 2229.9
Burnt clay 4 Bc 1.0–4 91.4 162.5 154 2240.0
8 Bc 1.0–8 182.8 93 153 2292.5
12 Bc 1.0–12 274.2 49 156 2286.1
Fly ash 4 Fa 1.0–4 91.4 180 160 2190.4
8 Fa 1.0–8 182.8 60 159 2239.5
12 Fa 1.0–12 274.2 15 153 2252.5
Ms: 1.2 Pumice 4 Pm 1.2–4 450 1215 104.7 175 155 2172.8
8 Pm 1.2–8 209.4 108 152 2176.3
12 Pm 1.2–12 314.1 49 152 2195.7
Perlite 4 Pr 1.2–4 104.7 145 151 2168.5
8 Pr 1.2–8 209.4 88 158 2215.7
12 Pr 1.2–12 314.1 26 153 2232.0
Burnt clay 4 Bc 1.2–4 104.7 148 156 2244.0
8 Bc 1.2–8 209.4 81 156 2268.0
12 Bc 1.2–12 314.1 16 153 2288.3
Fly ash 4 Fa 1.2–4 104.7 150 150 2184.5
8 Fa 1.2–8 209.4 40.5 153 2228.8
12 Fa 1.2–12 314.1 5.5 157 2219.7
Ms: 1.6 Pumice 4 Pm 1.6–4 450 1215 133.1 165 155 2142.1
8 Pm 1.6–8 266.2 60 151 2160.5
12 Pm 1.6–12 399.3 0 152 2191.7
Perlite 4 Pr 1.6–4 133.1 127 155 2164.5
8 Pr 1.6–8 266.2 42 153 2191.7
12 Pr 1.6–12 399.3 0 160 2212.5
Burnt clay 4 Bc 1.6–4 133.1 132 156 2188.5
8 Bc 1.6–8 266.2 49 152 2213.9
12 Bc 1.6–12 399.3 0 163 2261.9
Fly ash 4 Fa 1.6–4 133.1 140 158 2165.9
8 Fa 1.6–8 266.2 12 153 2190.4
12 Fa 1.6–12 399.3 0 200+ 2190.9
Ms: 2.0 Pumice 4 Pm 2.0–4 450 1215 160 150 154 2123.2
8 Pm 2.0–8 320 24 157 2164.5
12 Pm 2.0–12 480 0 200+ 2169.3
Perlite 4 Pr 2.0–4 160 112 155 2212.3
8 Pr 2.0–8 320 14 158 2213.6
12 Pr 2.0–12 480 0 200+ 2164.8
Burnt clay 4 Bc 2.0–4 160 120 157 2262.9
8 Bc 2.0–8 320 0 155 2291.2
12 Bc 2.0–12 480 0 200+ 2213.1
Fly ash 4 Fa 2.0–4 160 124 152 2160.3
8 Fa 2.0–8 320 7 153 2186.1
12 Fa 2.0–12 480 0 200+ 2173.1
a
As: aluminosilicate, Pm: pumice, Pr: perlite, Bc: burnt clay, Fa: fly ash.

4
A. Gultekin and K. Ramyar
Fig. 4. Compressive strength of burnt clay geopolymers oven-cured at a) 60◦ C for 72 h, b) 90◦ C for 48 h, c) 120◦ C for 24 h.
containing 4% and 8% Na2O increased with the increase of the Ms ratio
when cured at 90 or 120◦ C. In mortars containing 12% Na2O, on the
other hand, as the Ms ratio increased, the compressive strength
increased up to an optimum point, beyond which the strength reduced.
The general trend for the strength of pumice- and perlite-based mortars
cured at 90 and 120◦ C was similar, i.e., with increasing Ms ratio, the
compressive strength first increased and then decreased after an opti­
mum point. When the effect of the Na2O content of the activator (having
a definite Ms ratio) on the compressive strength was examined, it was
observed that the compressive strength generally increased with the
increase in the Na2O content from 4% to 8%. However, further increase
5
Ceramics International xxx (xxxx) xxx
in Na2O content to 12% reduced the strength. The reasons for these
observations are discussed in detail in the following paragraphs. 120◦ C-
24 h curing regime provided 23.6–29.1 MPa compressive strength in
these mixtures. Meanwhile, the most suitable activator characteristics
for the highest compressive strength were found to be 1.6 Ms ratio and
8% Na2O content for the pumice and perlite geopolymers, as well as 2.0
Ms ratio and 8% Na2O content for the burnt clay geopolymer mortar.
When the fly ash-based geopolymer mortars were examined, it was
observed that regardless of the curing regime and activator Ms ratio, the
compressive strengths of the mortars produced with 4% Na2O were close
to each other and below 10 MPa. The fact most probably arises from the
A. Gultekin and K. Ramyar
Fig. 5. Compressive strength of pumice and perlite geopolymers oven-cured at a) 60◦ C for 72 h, b) 90◦ C for 48 h, c) 120◦ C for 24 h.
low solubility of aluminum and silicon species in such an activator. The
compressive strengths increased with the increase of Ms ratio from 1.0 to
1.2 in the mortars produced with 8% Na2O activator at all three curing
temperatures. However, further increase in Ms ratio reduced the
strengths. The strength reduced gradually upon increasing the Ms ratio
at 12% Na2O content in the mortars produced with 1.0 Ms ratio. Using
the optimum Ms ratio (1.0) and Na2O content (12%) compressive
strengths of 54.4, 66.1 and 42.2 MPa were obtained at 60, 90 and 120◦ C
curing temperatures, respectively. There are numerous studies on the
effects of factors such as Ms ratio (hence the sodium silicate/sodium
hydroxide ratio), activator Na2O content, and Si/Al ratio of the alumi­
nosilicate on the compressive strength of geopolymer. Cho et al. [29]
explained that increasing the percentage of Na2O at a given Ms ratio
increased the compressive strength. The fact was attributed to the
increased solubility of the aluminosilicate compounds in the high
alkaline solution. However, Na2O content of the activator beyond a
certain level slowed down the polymerization. This caused precipitation
of the geopolymer gel on the surface of base material particles creating a
barrier against the contact of the activator and base material. Duxson
et al. [30] found that with the increase in Si/Al ratio, the strength firstly
increased and then decreased after an optimum value. Researchers
6
Ceramics International xxx (xxxx) xxx
stated that after a certain amount of Si/Al ratio, the number of unreacted
particles, acting as local defects, increased. These defects created stress
concentrations and reduced the strength by facilitating the collapse of
the matrix. Morsy et al. [31], Hanafiah et al. [32] and
Doğan-Sağlamtimur et al. [33] reported that increasing of the sodium
silicate/sodium hydroxide ratio in the alkali solution up to a certain
level, increased the compressive strength. Morsy et al. also stated that
the increase in the amount of SiO2 in the activator solution makes it
difficult for the water in the geopolymer to evaporate. Therefore, for­
mation of the geopolymer structure and the development of compressive
strength begin to reduce after an optimum SiO2 value.
The mixtures showing the highest strength (Pm 1.6-8-120◦ C, Pr 1.6-
8-120◦ C and Bc 2.0-8-120◦ C) were selected for microwave curing, SEM/
EDS, XRD, FT-IR, TG analysis and energy consumption comparison. The
highest strength in fly ash-based geopolymer was obtained in Fa 1.0-12-
90◦ C specimens. However, Fa 1.0-12-60◦ C specimens were preferred, as
they can be produced with a slightly lower energy consumption, being
more suitable for applications such as on-site casting/prefabrication.
A. Gultekin and K. Ramyar
Fig. 6. Compressive strength of fly ash geopolymer mortars oven-cured at a) 60◦ C for 72 h, b) 90◦ C for 48 h, c) 120◦ C for 24 h.
3.2. Microwave curing
The compressive strength of microwave-cured mortars is shown in
Fig. 7. In general, irrespective of the curing time and microwave power,
the strengths of fly ash-based mortars are close to each other and in the
range of 16.1–24.0 MPa. In samples cured at 450 W, the compressive
strength increased with the increase in curing time. Opposite results
were found in the 600 and 800 W curing regimes. The strength of
microwave-cured pumice, perlite and burnt clay geopolymer mortars
generally increased with increasing curing time at 450 and 600 W. The
strength of these mixtures reduced at 800 W with the increasing curing
7
Ceramics International xxx (xxxx) xxx
time. Graytee et al. [18] reported that the strengths increased with the
increase of the curing time at the same power level. The researchers also
examined the effect of change in power level on the compressive
strength and showed that the geopolymer strength increased by 22% as
the microwave power increased from 200 W to 300 W. Beyond this
power level, however, the strengths gradually decreased. The authors
stated the following probable reasons for the fact. The increase in the
power level, causing rapid evaporation of water, leaves no water
required for polymerization. Moreover, microcracks form due to the
rapid evaporation of the water. Finally, local hot spots form due to the
differences in the dielectric properties of the materials in the mixture
A. Gultekin and K. Ramyar Ceramics International xxx (xxxx) xxx

Fig. 7. Compressive strength of microwave-cured a) pumice, b) perlite, c) burnt clay, d) fly ash geopolymers.

causing high internal stresses and deterioration. El-Feky et al. [20]
similarly stated that microwave curing accelerated the geo­
polymerization process. However, during the curing at the same power
level, with the increasing curing time the temperature of the specimen
increased, resulting in accelerated polycondensation, which also caused
earlier formation of the gel. The gel thus formed prevented the
dissolution of unreacted alumina and silica species in the aluminosili­
cate. Since the increase in curing time increases the temperature of the
specimen, it accelerates the evaporation of the pore solution and causes
incomplete geopolymerization. The researchers stated that prolonging
the curing beyond a certain time damages the geopolymer structure,
causes dehydration in the matrix and increases the shrinkage reducing

8
A. Gultekin and K. Ramyar Ceramics International xxx (xxxx) xxx

strength. Tan et al. [21] studied microwave curing of metakaolin

substituted recycled aggregate powder-based geopolymers. It was stated
that a certain microwave curing time activates more aluminosilicate
particles and results in a denser gel. However, due to the increase in
temperature, the rapid evaporation of water from the dense geopolymer
structure with limited expansion capacity causes cracking.
In spite of the fly ash geopolymers where short microwave curing
time was not sufficient to promote the strength to a desired level, the
pumice-, perlite- and burnt clay-based mortars upon microwave curing
achieved even 5.7–54.7% higher strength than that of their oven-cured
counterpart specimens. The fact was more pronounced in the perlite
geopolymers. Somaratna et al. [19] applied oven curing (at 75◦ C for 48
h) and microwave curing (240 W for 120 min) on the alkali activated fly
ash mortars with 6, 8, 10 M activators and reported the superiority of the
microwave curing in terms of strength.
According to Graytee et al. [18], an effective microwave curing can
increase the strength gain rate by providing a rapid and uniform heating
effect. The researcher stated that in the conventional curing, heat
transfers into the sample with conduction, radiation and convection, but
in the microwave curing, waves create uniform heating in the entire
volume. El-Feky et al. [20] stated that conventional heating is slow due
to the slow transfer of heat from the sample surface to the core, resulting
in a non-uniform heat distribution in various parts of the specimen.
However, in the microwave curing, energy is transferred to the sample
electromagnetically, rather than in the form of thermal heat flux, so that
Fig. 8. Fracture pattern of a geopolymer sample (Pm-1.6-8-120◦ C-24 h) with
a homogeneous heat distribution is achieved throughout the specimen.
26.3 MPa compressive strength.
According to Somaratna et al. [19] the reason for the higher rate of
strength development and greater strength in the microwave-cured
structure. However, increasing the Na2O ratio to 8%, improved the in­
geopolymers than those of oven-cured counterparts is the uniform
ternal structure and reduced the number of voids and unreacted parti­
microstructure arisen from the uniform heating provided by the mi­
cles with a consequent increase in strength. In the fly ash-based
crowave curing. Oppositely, non-uniform heat distribution and differ­
geopolymer pastes, a similar situation was observed with the decrease of
ential thermal stresses within the specimen during oven curing result in
the Ms ratio at a given Na2O ratio. The microstructure of microwave-
a non-uniform internal structure lowering the strength. From the results
cured pumice, perlite and burnt clay pastes were found to be similar
obtained in this study, it can be concluded that the uniform heating and
to those of their oven-cured counterparts. However, the internal struc­
absence of thermal gradient in the microwave-cured pumice, perlite,
ture of oven-cured fly ash paste was much denser and more homoge­
and burnt clay-based geopolymer specimens is the reason for their
neous than that of the microwave-cured one. The 2.3 times difference in
higher strength than their counterpart specimens cured in the oven. On
strength of microwave- and oven-cured fly ash mortars clearly demon­
the other hand, the reason for the low strength of the microwave-cured
strates the effect of the internal structure on the strength of mixture.
fly ash-based specimens than their oven-cured ones is in the lower
The results of EDS analysis reported in Table 3 were obtained on
dissolution of fly ash particles in the activator solution due to the
random points representing the overall paste characteristic. The re­
shortness of microwave curing time. The fact also revealed from the SEM
ported values are the average of at least 2 points. According to the re­
images of microwave-cured fly ash samples in which an excessive
sults, the pastes mainly consist of oxygen, silicon, aluminum, and
amount of undissolved fly ash particles were observed.
sodium atoms. However, Si/Al, Na/Al and Si/Na ratios are quite
The optimum microwave curing regime for pumice geopolymer was
different in the various pastes.
found to be 600 W-15 min, while 450 W-15 min microwave curing
resulted in the highest strengths in the perlite, burnt clay and fly ash
mixtures. The fact perhaps arises from the high water content of pumice 3.4. TGA results
mixtures which requires greater energy for evaporation.
When the fracture patterns of the samples were examined, it was Numerous studies have been conducted on the weight loss in TG
observed that, regardless of the curing type, the samples with less than analysis of geopolymers. Das and Rout [34] and Hassan et al. [35] stated
8–10 MPa compressive strength were crushed completely to the smith­ that the sudden weight loss in the range of 0–200◦ C was caused by the
ereens. However, the samples with >10 MPa strength showed fracture free and weakly bonded-absorbed water in the fly ash geopolymers.
patterns (not completely in pieces) similar to those of the portland Hong and Kim [36] reported that the main causes of TGA weight loss of
cement mortars with similar strengths (Fig. 8). Moreover, stronger the fly ash geopolymers in three different temperature zones (0–120,
samples crushed in a more brittle manner than those with lower 120–350 and above 350◦ C) are different. The main reasons for the
strength. weight loss in the first and second zone are the loss of physically
adsorbed water and evaporation of the chemically bonded water,
3.3. SEM/EDS analysis respectively. At temperatures above 350◦ C dehydroxylation, and above
430◦ C combustion of the calcium compounds and unburned carbon are
The SEM views of selected oven-cured and microwave-cured pastes responsible too for the weight loss. Yang et al. [37] stated that the
are shown in Figs. 9–12. In these figures the unreacted and partially weight loss below 400◦ C is due to free water and structural water loss,
reacted aluminosilicate particles are shown in the yellow and orange while the weight loss between 400 and 800◦ C arises from the slow and
circles, respectively. It was observed that the internal structure of the progressive dehydroxylation between the geopolymer chains or the re­
oven-cured burnt clay, pumice and perlite geopolymers changed with actions that occur to form new oligomers in the matrix. Liu et al. [38]
increasing the activator Na2O ratio. The mixtures containing 4% Na2O claimed that the weight losses in TG analysis of the metakaolin geo­
had large voids, many unreacted particles and an inhomogeneous polymers between 25-110◦ C and 110–265◦ C are due to free water and

9
A. Gultekin and K. Ramyar Ceramics International xxx (xxxx) xxx

Fig. 9. Oven-cured pumice pastes a) 1.6-4-120◦ C, b) 1.6-8-120◦ C and microwave-cured pumice pastes c) 1.6-8-450W-5 min, d) 1.6-8-600W-15 min.

Fig. 10. Oven-cured perlite pastes, a) 1.6-4-120◦ C, b) 1.6-8-120◦ C and microwave-cured perlite pastes, c) 1.6-8-450W-5 min, d) 1.6-8-450W-15 min.

10
A. Gultekin and K. Ramyar Ceramics International xxx (xxxx) xxx

Fig. 11. Oven-cured burnt clay pastes a) 2.0-4-120◦ C, b) 2.0-8-120◦ C and microwave-cured burnt clay pastes c) 2.0-8-450W-5 min, d) 2.0-8-450W-15 min.

Fig. 12. Oven-cured fly ash pastes a) 1.6-12-60◦ C, b) 1.0-12-60◦ C and microwave-cured fly ash pastes c) 1.0-12-450W-5 min, d) 1.0-12-450W-15 min.

11
A. Gultekin and K. Ramyar Ceramics International xxx (xxxx) xxx

Table 3 200–500◦ C is due to the chemically bonded water. The weight loss
EDS analysis results of geopolymer pastes. beyond 500◦ C seems to be due to the loss of unburned carbon and
Code % (by atom) chemically bond water. However, during the preparation of the paste
majority of the unburned coal particles were collected on the top of the
Si Al Na K O Ca Mg Fe
specimen which were probably removed from the sample during fin­
Pm 1.6-8- 22.87 4.27 8.70 2.10 61.15 0.25 0.32 0.31 ishing. Therefore, the impact of unburned coal on TGA of pastes is
120◦ C-
24 h
limited. The microwave-cured geopolymer paste lost greater weight
Pr 1.6-8- 21.14 4.95 4.45 1.73 66.82 0.23 0.47 0.22 than that of the oven-cured one. This can be attributed to the lower
120◦ C- amount of water evaporated during 15-min curing of the microwave
24 h sample than that of the oven-cured one cured for a much longer period.
Bc 2.0-8- 18.62 6.38 5.47 0.08 68.75 0.14 0.46 0.12
The TG weight loss graphs of burnt clay and its oven- and
120◦ C-
24 h microwave-cured geopolymer pastes are shown in Fig. 14. The burnt
Fa 1.0-12- 15.86 5.22 13.69 0.41 62.15 1.38 0.78 0.53 clay did not experience a significant weight loss up to approximately
60◦ C-72 460◦ C, and there was a considerable weight loss in the range of
h 460–700◦ C. It is thought that the weight loss in this temperature range is
Pm 1.6-8- 23.52 4.99 5.71 2.01 62.99 0.26 0.34 0.20
600W-
due to the evaporation of the interlayer water and some chemically
15min combined water of the clay. Burnt clay geopolymer pastes showed a
Pr 1.6-8- 20.12 4.20 5.46 0.84 68.63 0.19 0.44 0.16 progressive linear weight loss up to 700◦ C with a similar trend. The
450W- weight loss of these pastes beyond 700◦ C was negligible.
15min
The TG weight loss graphs of raw pumice, raw perlite and their oven/
Bc 2.0-8- 18.14 8.35 6.17 0.09 66.74 0.12 0.27 0.13
450W- microwave-cured geopolymer pastes are shown in Figs. 15 and 16,
15min respectively. None of these samples experienced a sudden loss of weight.
Fa 1.0-12- 21.16 12.73 7.26 0.56 53.45 1.83 1.23 1.80 The samples showed a slow and progressive loss of weight up to 600◦ C.
450W- The weight loss of these geopolymer pastes and raw materials was not
15min
remarkable beyond 600◦ C. While the weight loss curves of the micro­
wave- and oven-cured perlite geopolymers were very similar to each
physically bonded water loss, respectively. The loss of physico-chemical other, the weight loss in microwave-cured pumice geopolymers was very
bonded water, as well as dihydroxylation/polycondensation processes low. The weight loss up to 200◦ C is due to the evaporation of the free
between 270 and 630◦ C are the main reasons of the weight loss in this water and weak physically combined water. The weight loss of pumice
temperature range. and perlite pastes at 200–600◦ C arises from the loss of water from these
Weight loss graphs of the (raw) fly ash as well as its oven- and aluminosilicates. This is evident from the loss of weights of these ma­
microwave-cured geopolymer pastes are shown in Fig. 13. There was no terials in the raw state. Almalkawi et al. [39] found 7% weight loss in TG
considerable weight loss in the raw fly ash up to 500◦ C. Beyond this analysis of ground raw pumice up to 900◦ C. The majority of this
temperature, there was a weight loss arisen probably from the unburned happened at temperatures up to 550◦ C. According to these researchers
carbon. It should be noted that the loss on ignition of the fly ash which is pumice is a hydrophilic material containing considerable water. The
a measure of its unburned carbon is 17%. However, since TG analysis is weight loss of pumice arises majorly from the loss of free water as well as
carried out on very small (20–40 mg) samples, it seems that the small loss of water from the Si–OH, Al–OH groups. Cetintas [40], on the other
sample is not a good representative of the material in terms of unburned hand, experienced most of the weight loss in the TG analysis of perlite at
carbon. Geopolymer pastes showed a considerable weight loss up to temperatures up to 600–650◦ C. In the present study the
200◦ C arisen from the loss of free water. The weight loss in the range of microwave-cured pumice sample showed much less weight loss than the

Fig. 13. TGA of raw fly ash and fly ash-based geopolymer pastes.

12
A. Gultekin and K. Ramyar Ceramics International xxx (xxxx) xxx

Fig. 14. TGA of raw burnt clay and burnt clay-based geopolymer pastes.

Fig. 15. TGA of ground raw pumice and pumice-based geopolymer pastes.

other samples. The fact was attributed to the curing of this sample at located between about 900 and 1100 cm− 1, were due to the Si–O–Al and
600 W which resulted in a considerable water loss during the curing. Si–O–Si asymmetric stretching vibrations. According to Criado et al.
[41], the shift of the wide and large band around 1078 cm− 1 in the raw
fly ash to lower wave numbers in the geopolymer samples was arisen
3.5. FT-IR and XRD
from the formation of sodium aluminosilicate hydrate gel. Azevedo et al.
[43] attributed this shift to the formation of the three-dimensional
Fig. 17 shows the FT-IR spectra of geopolymer pastes and raw alu­
framework containing silicon and aluminum tetrahedra. The re­
minosilicates. Criado et al. [41] stated that the bands around 460 cm− 1
searchers emphasized that the newly formed structure upon geo­
and 1078 cm− 1 are associated with the bending vibrations of the T-O-T
polymerization, named as N-A-S-H gel, is the reason for the binding
bonds, and the asymmetric stretching vibrations of T-O, respectively (T:
property and mechanical strength of the material. In this study, the band
Si or Al). These two broad and intense bands are characteristic of TO4
peaking at 1085 cm− 1 in the raw fly ash shifted to around 1001-1032
tetrahedra structure. The bands around 1150, 1084, 796-778, 697, 668,
cm− 1 upon geopolymerization. Similar shifts were observed in the
522 and 460 cm− 1 are attributed to the quartz, whereas the peaks
pumice-based matrix (from 1050 to 1012-1042 cm− 1), in the
around 1130-1180 cm− 1 and 550-560 cm− 1 to the presence of mullite in
perlite-based matrix (from 1050 to 1046-1042 cm− 1), and in the burnt
the raw fly ash. Toniolo et al. [42] stated that the wide and large band,

13
A. Gultekin and K. Ramyar Ceramics International xxx (xxxx) xxx

Fig. 16. TGA of ground raw perlite and perlite-based geopolymer pastes.

Fig. 17. FT-IR spectra of geopolymer pastes and raw aluminosilicates.

clay-based matrix (from 1119 to 1081-1085 cm− 1).
The number of studies on perlite- and pumice-based geopolymers
and their FT-IR spectra is limited. Erdogan [44] and Taxiarchou et al.
[27] stated that the vibrations seen at the wave number range of
800–1300 cm− 1 originates from both the amorphous and crystalline
phases in the raw perlite. In the raw perlite, the two peaks at 1030 and
1135 cm− 1 were attributed to the asymmetric stretching vibration of
Si–O–Si and Si–O–Si/Si–O–Al, respectively [44,45]. Taxiarchou et al.
[27] detected that the band located around 1043 cm− 1 in the raw perlite
shifted to around 1030 cm− 1 in the perlite-based matrix with geo­
polymeriation. The fact was attributed to the increase in tetrahedral Al
substitution in the geopolymeric network and the incorporation of Si

14
A. Gultekin and K. Ramyar
Fig. 18. XRD spectra of geopolymer pastes and raw aluminosilicates (q: quartz, s: sanidine, a: albite, d: dickite, k: kaolinite, m: mullite, h: hematite, ms: muscovite,
z: zeolite).
and Al species into the geopolymeric network structure. Erdogan [44]
reported that this shift can be considered as an indication of the geo­
polymerization and the intensity of the band around 460 cm− 1, attrib­
uted to O–Si–O and Si–O–Si bending vibrations, was found to be less in
the geopolymer samples due to the change of the raw perlite structure
with geopolymerization. Tasdelen [46] assigned the peaks around 460
and 780 cm− 1 to the bending vibrations of Si–O–Si bonds in the raw
pumice. In the present study, with geopolymerization, the wide and
intense peaks around 1050 cm− 1 in the raw perlite and pumice were
observed to be shifted to the lower wave numbers. This was also the case
in fly ash-based system.
Tironi et al. [47] stated that if all four of the bands at 3620, 3650,
3670 and 3700 cm− 1 in the FT-IR spectrum of kaolinite are clearly seen,
the kaolinite structure is ordered, while the disappearance of the band at
3670 cm− 1 indicates that the structure is disordered and prone to easy
dehydration. Moreover, the bands seen around 430, 470, 1009, 1032,
1115 cm− 1 were reported to be associated with the Si–O bonds, the
bands around 538, 754, 789 cm− 1 to the Si–O–Al bonds and the bands
around 696, 912, 939 cm− 1 to the Al–OH bonds. Nmiri et al. [48]
attributed the peak at 798 cm− 1 in the raw metakaolin to the Si–O bond
vibrations, stating that the intensity of this band may decrease with
geopolymerization. The fact arises from the reduction of aluminum co­
ordination from VI to IV, which characterizes the geopolymer structure.
The appearance of this band in geopolymer samples was related to the
presence of the unreacted metakaolin particles [48].
Regarding the FT-IR spectra of the materials used in the present
study, the peaks around 3400-3500 cm− 1 were attributed to the –OH
and H–O–H stretching vibrations [42,49], while the peaks around
1600-1650 cm− 1 wave numbers to the H–O–H bending vibrations [42,
50]. These seem to be caused by the water or –OH ions in the sample or
on its surface. Several researchers reported that the peaks around
1400-1450 cm− 1 were associated with the carbonates in the geopolymer
[51,52]. Toniolo et al. [42] observed the band originating from
15
Ceramics International xxx (xxxx) xxx
carbonation at around 1430 cm− 1 and stated that this band is linked
with the O–C–O stretching vibrations of the carbonates formed by the
interaction of unreacted activator in the geopolymer with the CO2 of air.
Examination of the XRD spectra of geopolymer pastes and raw alu­
minosilicates, shown in Fig. 18, revealed the presence of dickite, quartz
and kaolinite peaks in the burnt raw clay. On the other hand, sanidine,
albite and quartz peaks were detected in the raw pumice and perlite.
Besides, there was some changes in the peak intensities after geo­
polymerization of the burnt clay-, pumice- and perlite-based geo­
polymer pastes. In addition, new peaks were formed in the pumice and
perlite-based geopolymers after 15 min of microwave curing. This sit­
uation was more clear in the fly ash-based geopolymers. In place of
mullite, muscovite, hematite and quartz peaks found in the XRD spec­
trum of raw fly ash, several zeolite peaks were appeared in the spectrum
of 15-min microwave-cured fly ash geopolymer. Similar observations
were made on the fly ash-based geopolymers by Shi et al. [22] and
Bakharev [53] to report the formation of zeolitic structures in these
mixtures.
3.6. Energy consumption during curing
The amount of energy required to precure/cure the specimens
(consumed either by the conventional oven and/or by the microwave
oven) as well as their compressive strengths are shown in Table 4. As can
be seen from the table, irrespective of the aluminosilicate material type,
the electricity consumption per unit compressive strength is consider­
ably low in the microwave curing. In pumice, perlite and clay-based
geopolymers, microwave curing, in spite of consuming less energy,
resulted in a higher compressive strength than the oven curing. These
results show that reasonable compressive strengths can be achieved with
a short microwave curing time and low energy consumption.
A. Gultekin and K. Ramyar Ceramics International xxx (xxxx) xxx

Table 4
Energy consumption during curing of selected geopolymer mortar mixtures.
Mixture Comp. strength (MPa) Energy consumption (kWh) Energy cons./MPa Energy saving (%)

Precure (oven) Oven curing Microwave curing Total

Pm 1.6-8-120◦ C-24 h 26.3 – 8.90 – 8.90 0.338

80.2
Pm 1.6-8-600W-15min 27.8 1.59 – 0.27 1.86 0.067
Pr 1.6-8-120◦ C-24 h 23.6 – 8.90 – 8.90 0.377
87.0
Pr 1.6-8-450W-15min 36.5 1.59 – 0.21 1.80 0.049
Bc 2.0-8-120◦ C-24 h 29.1 – 8.90 – 8.90 0.306
86.3
Bc 2.0-8-450W-15min 33.6 1.21 – 0.21 1.42 0.042
Fa 1.0-12-60◦ C-72 h 54.4 – 12.62 – 12.62 0.231
77.1
Fa 1.0-12-450W-15min 24.0 1.05 – 0.21 1.26 0.053

4. Conclusions Acknowledgment

In this study, the effect of microwave and oven curing on the pumice,
perlite, burnt clay and fly ash-based geopolymer mortars was investi­
gated. For this purpose, alkali solutions having four different Ms ratios
(1.0, 1.2, 1.6, and 2.0) and three different Na2O ratios by weight of
aluminosilicate (4, 8, and 12%) were used. For the materials used and
tests applied the following conclusions were drawn:
This work was supported by The Scientific and Technological
Research Council of Turkey (TUBITAK) [grant number 119M950]. The
authors also acknowledge the contribution of Ege University Central
Research, Test and Analysis Laboratory for SEM/EDS & TG analysis and
Izmir Katip Celebi University Central Research Laboratory for XRD and
FT-IR analysis as well as particle size distribution determination.

• It is possible to produce medium strength (around 25 MPa) geo­ References

polymer building materials with natural pozzolans (perlite-pumice)
using oven curing.
• Compared to the strength of oven-cured counterpart mixtures, even
15 min microwave curing increased the strength of pumice, perlite
and burnt clay mortars by 5.7%, 54.7% and 15.5%, respectively.
• Microwave–cured fly ash-based geopolymer mortars were produced
in short curing times, but strengths higher than 24 MPa cannot be
obtained.
• During TGA neither the oven-cured nor the microwave-cured geo­
polymer pastes showed rapid weight loss at high temperatures
beyond 100◦ C. The maximum TGA weight loss recorded in the
geopolymer pastes was 15.5%.
• SEM observations confirmed the similarity of microstructure of
microwave-cured perlite, pumice and burned clay-based geo­
polymers to those of their oven-cured counterparts.
• New peaks were detected in the X-ray difractograms of pumice and
perlite-based geopolymers after 15 min of microwave curing. The
fact was more clear in the fly ash-based geopolymer by the appear­
ance of several zeolite peaks.
• The wide and large bands in the FT-IR spectra of the aluminosilicates
at around 1050 to 1119 cm− 1 were shifted to lower wavenumbers
upon geopolimerization. The signs of the presence of water, –OH ions
and carbonates were detected in the FT-IR spectra of the geopolymer
pastes.
• The microwave-cured pumice, perlite, and burned clay geopolymers
provided significant energy savings along with equivalent or greater
strength than that of the oven-cured counterparts.
• For the unit compressive strength microwave curing of pumice,
perlite, burnt clay and fly ash mortars resulted in 80.2, 87.0, 86.3 and
77.1% lower energy consumption than the oven curing, respectively.
CRediT authorship contribution statement
Adil Gultekin: Conceptualization, Experimentation, Methodology,
Writing – original draft. Kambiz Ramyar: Conceptualization, Method­
ology, Writing – review & editing, Supervision.
Declaration of competing interest
The authors declare that they have no known competing financial
interests or personal relationships that could have appeared to influence
the work reported in this paper.
[1] J. Cai, J. Pan, X. Li, J. Tan, J. Li, Electrical resistivity of fly ash and metakaolin
based geopolymers, Construct. Build. Mater. 234 (2020) 117868, https://doi.org/
10.1016/j.conbuildmat.2019.117868.
[2] M.B. Ali, R. Saidur, M.S. Hossain, A review on emission analysis in cement
industries, Renew. Sustain. Energy Rev. 15 (2011) 2252–2261, https://doi.org/
10.1016/j.rser.2011.02.014.
[3] A.M. Aly, M.S. El-Feky, M. Kohail, E.S.A.R. Nasr, Performance of geopolymer
concrete containing recycled rubber, Construct. Build. Mater. 207 (2019) 136–144,
https://doi.org/10.1016/j.conbuildmat.2019.02.121.
[4] F. Cao, M. Meng, B. Shan, R. Sun, Source apportionment of mercury in surface soils
near the Wuda coal fire area in Inner Mongolia, China, Chemosphere 263 (2021)
128348, https://doi.org/10.1016/j.chemosphere.2020.128348.
[5] A.C. Ganesh, M. Muthukannan, Development of high performance sustainable
optimized fiber reinforced geopolymer concrete and prediction of compressive
strength, J. Clean. Prod. 282 (2021) 124543, https://doi.org/10.1016/j.
jclepro.2020.124543.
[6] V. Shobeiri, B. Bennett, T. Xie, P. Visintin, A comprehensive assessment of the
global warming potential of geopolymer concrete, J. Clean. Prod. 297 (2021)
126669, https://doi.org/10.1016/j.jclepro.2021.126669.
[7] J. Cai, J. Tan, X. Li, Thermoelectric behaviors of fly ash and metakaolin based
geopolymer, Construct. Build. Mater. 237 (2020) 117757, https://doi.org/
10.1016/j.conbuildmat.2019.117757.
[8] P. Duxson, J.L. Provis, G.C. Lukey, J.S.J. van Deventer, The role of inorganic
polymer technology in the development of ‘green concrete, Cement Concr. Res. 37
(12) (2007) 1590–1597, https://doi.org/10.1016/j.cemconres.2007.08.018, 2007.
[9] X. Jiang, Y. Zhang, R. Xiao, P. Polaczyk, M. Zhang, W. Hu, Y. Bai, B. Huang,
A comparative study on geopolymers synthesized by different classes of fly ash
after exposure to elevated temperatures, J. Clean. Prod. 270 (2020) 122500,
https://doi.org/10.1016/j.jclepro.2020.122500.
[10] W.P. Zakka, N.H.A.S. Lim, M.C. Khun, A scientometric review of geopolymer
concrete, J. Clean. Prod. 280 (1) (2021) 124353, https://doi.org/10.1016/j.
jclepro.2020.124353.
[11] R. Firdous, D. Stephan, Effect of silica modulus on the geopolymerization activity
of natural pozzolans, Construct. Build. Mater. 219 (2019) 31–43, https://doi.org/
10.1016/j.conbuildmat.2019.05.161, 2019.
[12] R.A. Robayo-Salazar, R.M. de Gutierrez, Natural volcanic pozzolans as an available
raw material for alkali-activated materials in the foreseeable future: a review,
Construct. Build. Mater. 189 (2018) 109–118, https://doi.org/10.1016/j.
conbuildmat.2018.08.174, 2018.
[13] T. Suwan, B. Paphawasit, M. Fan, P. Jitsangiam, P. Chindaprasirt, Effect of
microwave-assisted curing process on strength development and curing duration of
cellular lightweight geopolymer mortar, Mater. Manuf. 36 (9) (2021) 1040–1048,
https://doi.org/10.1080/10426914.2021.1885702.
[14] International Energy Agency, Global share of electricity generation in 2018. htt
ps://www.iea.org/data-and-statistics/charts/global-share-of-electricity-generatio
n-2018, 2018. (Accessed 1 October 2021).
[15] S. Sun, W. Liu, W. Guan, S. Zhu, J. Jia, X. Wu, R. Lei, T. Jia, Y. He, Effects of air
pollution control devices on volatile organic compounds reduction in coal-fired
power plants, Sci. Total Environ. 782 (2021) 146828, https://doi.org/10.1016/j.
scitotenv.2021.146828.
[16] J. Luo, O. Emelogu, T. Morosuk, G. Tsatsaronis, Exergy-based investigation of a
coal-fired allam cycle, Energy 218 (2021) 119471, https://doi.org/10.1051/
e3sconf/201913701018.
[17] S. Suman, Hybrid nuclear-renewable energy systems: a review, J. Clean. Prod. 181
(2018) 166–177, https://doi.org/10.1016/j.jclepro.2018.01.262.

16
A. Gultekin and K. Ramyar
[18] A. Graytee, J.G. Sanjayan, A. Nazari, Development of a high strength fly ash-based
geopolymer in short time by using microwave curing, Ceram. Int. 44 (7) (2018)
8216–8222, https://doi.org/10.1016/j.ceramint.2018.02.001.
[19] J. Somaratna, D. Ravikumar, N. Neithalath, Response of alkali activated fly ash
mortars to microwave curing, Cement Concr. Res. 40 (12) (2010) 1688–1696,
https://doi.org/10.1016/j.cemconres.2010.08.010.
[20] M.S. El-Feky, M. Kohail, A.M. El-Tair, M.I. Serag, Effect of microwave curing as
compared with conventional regimes on the performance of alkali activated slag
pastes, Construct. Build. Mater. 233 (2020) 117268, https://doi.org/10.1016/j.
conbuildmat.2019.117268.
[21] J. Tan, J. Cai, L. Huang, Q. Yang, M. Mao, J. Li, Feasibility of using microwave
curing to enhance the compressive strength of mixed recycled aggregate powder
based geopolymer, Construct. Build. Mater. 262 (2020) 120897, https://doi.org/
10.1016/j.conbuildmat.2020.120897.
[22] S. Shi, H. Li, M. Fabian, T. Sun, K.T.V. Grattan, D. Xu, P.A.M. Basheer, Y. Bai,
Alkali-activated fly ash manufactured with multi-stage microwave curing. Fourth
international conference on sustainable construction materials and technologies,
Las Vegas, USA (2016), https://doi.org/10.18552/2016/SCMT4S260.
[23] B.J. Kim, C.K. Yi, K.I. Kang, Characteristics of alkali-activated natural Hwangtoh
paste utilizing microwave heating, J. Korea Inst. Build. Constr. 12 (5) (2012)
503–509, https://doi.org/10.5345/JKIBC.2012.12.5.503.
[24] P. Chindaprasirt, U. Rattanasak, S. Taebuanhuad, Role of microwave radiation in
curing the fly ash geopolymer, Adv. Powder Technol. 24 (2013) 703–707, https://
doi.org/10.1016/j.apt.2012.12.005.
[25] S. Hong, H. Kim, Robust synthesis of coal bottom ash-based geopolymers using
additional microwave heating and curing for high compressive strength properties,
Kor. J. Chem. Eng. 36 (7) (2019) 1164–1171, https://doi.org/10.1007/s11814-
019-0286-y.
[26] TSE, TS EN 459-2: Building Lime - Part 2: Test Methods, 2011. Ankara, Turkey.
[27] M. Taxiarchou, D. Panias, C. Panagiotopoulou, A. Karalis, C. Dedeloudis, Study on
the suitability of volcanic amorphous aluminosilicate rocks (perlite) for the
synthesis of geopolymer-based concrete, in: L. Struble, J. Hicks (Eds.), STP1566-EB
Geopolymer Binder Systems, 2013, pp. 1–20, https://doi.org/10.1520/
STP156620120077. ASTM International.
[28] H. Kurt, Preparation of Geopolymers Using Inorganic Materials and Investigation
of the Effect of the Pumice on the Geopolymer, Master Thesis, Graduate School of
Natural and Applied Sciences, Cumhuriyet University, Sivas, Turkey, 2016.
[29] Y.K. Cho, S.W. Yoo, S.H. Jung, K.M. Lee, S.J. Kwon, Effect of Na2O content, SiO2/
Na2O molar ratio, and curing conditions on the compressive strength of FA-based
geopolymer, Construct. Build. Mater. 145 (2017) 253–260, https://doi.org/
10.1016/j.conbuildmat.2017.04.004.
[30] P. Duxson, J.L. Provis, G.C. Lukey, S.W. Mallicoat, W.M. Kriven, J.S.J. van
Deventer, Understanding the relationship between geopolymer composition,
microstructure and mechanical properties, Colloids Surf. A Physicochem. Eng. Asp.
269 (2005) 47–58, https://doi.org/10.1016/j.colsurfa.2005.06.060, 2005.
[31] M.S. Morsy, S.H. Alsayed, Y. Al-Salloum, T. Almusallam, Effect of sodium silicate to
sodium hydroxide ratios on strength and microstructure of fly ash geopolymer
binder, Arabian J. Sci. Eng. 39 (2014) 4333–4339, https://doi.org/10.1007/
s13369-014-1093-8, 2014.
[32] S. Hanafiah, D.O. Elysandi, D.G. Meykan, Effect of Na2SiO3/NaOH on mechanical
properties and microstructure of geopolymer mortar using fly ash and rice husk ash
as precursor, AIP Conf. Proc. 1903 (2017), 050013, https://doi.org/10.1063/
1.5011552.
[33] N. Dogan-Saglamtimur, H.O. Oz, A. Bilgil, T. Vural, E. Suzgec, The effect of alkali
activation solutions with different water glass/NaOH solution ratios on
geopolymer composite materials, IOP Conf. Ser. Mater. Sci. Eng. 660 (2019),
012003, https://doi.org/10.1088/1757-899X/660/1/012003.
[34] D. Das, P.K. Rout, Synthesis, Characterization and properties of fly ash based
geopolymer materials, Mater. Eng. 30 (2020) 3213–3231, https://doi.org/
10.1007/s11665-021-05647-x.
[35] A. Hassan, M. Arif, M. Shariq, Mechanical behaviour and microstructural
investigation of geopolymer concrete after exposure to elevated temperatures,
Arabian J. Sci. Eng. 45 (2020) 3843–3861, https://doi.org/10.1007/s13369-019-
04269-9.
17
Ceramics International xxx (xxxx) xxx
[36] S. Hong, H. Kim, Effects of microwave energy on fast compressive strength
development of coal bottom ash-based geopolymers, Sci. Rep. 9 (2019) 15694,
https://doi.org/10.1038/s41598-019-52160-2.
[37] Z. Yang, R. Mocadlo, M. Zhao, R.D. Sisson Jr., M. Tao, J. Liang, Preparation of a
geopolymer from red mud slurry and class F fly ash and its behavior at elevated
temperatures, Construct. Build. Mater. 221 (2019) 308–317, https://doi.org/
10.1016/j.conbuildmat.2019.06.034.
[38] X. Liu, J. Jiang, H. Zhang, M. Li, Y. Wu, L. Guo, W. Wang, P. Duan, W. Zhang,
Z. Zhang, Thermal stability and microstructure of metakaolin-based geopolymer
blended with rice husk ash, Appl. Clay Sci. 196 (2020) 105769, https://doi.org/
10.1016/j.clay.2020.105769.
[39] A.T. Almalkawi, S. Hamadna, P. Soroushian, One-part alkali activated cement
based volcanic pumice, Construct. Build. Mater. 152 (2017) 367–374, https://doi.
org/10.1016/j.conbuildmat.2017.06.139.
[40] R. Cetintas, Structure-property Relationship in Volcanic Ash Based One Part
Geopolymers and Perlite-Metakaolin Based Two Part Geopolymers, Master Thesis,
Institute of Graduate Studies in Science and Engineering. Bogazici University,
İstanbul, Turkey, 2018.
[41] M. Criado, A. Fernández Jiménez, I. Sobrados, A. Palomo, J. Sanz, Effect of relative
humidity on the reaction products of alkali activated fly ash, J. Eur. Ceram. Soc. 32
(2012) 2799–2807, https://doi.org/10.1016/j.jeurceramsoc.2011.11.036.
[42] N. Toniolo, G. Taveri, K. Hurle, J.A. Roether, P. Ercole, I. Dlouhy, A.R. Boccaccini,
Fly-ash-based geopolymers: how the addition of recycled glass or red mud waste
influences the structural and mechanical properties, J. Ceram. Sci. Technol. 8 (3)
(2017) 411–420, https://doi.org/10.4416/JCST2017-00053.
[43] A.G.S. Azevedo, K. Strecker, L.A. Barros, L.F. Tonholo, C.T. Lombardi, Effect of
curing temperature, activator solution composition and particle size in Brazilian
fly-ash based geopolymer production, Mater. Res. 22 (suppl.1) (2019), e20180842,
https://doi.org/10.1590/1980-5373-MR-2018-0842.
[44] S.T. Erdogan, Properties of ground perlite geopolymer mortars, J. Mater. Civ. Eng.
27 (7) (2015), 04014210, https://doi.org/10.1061/(ASCE)MT.1943-
5533.0001172.
[45] E.R. Vance, D.S. Perera, P. Imperia, D.J. Cassidy, J. Davis, J.T. Gourley, Perlite
waste as a precursor for geopolymer formation, J. Australas. Ceram. Soc. 45 (1)
(2009) 44–49.
[46] B. Tasdelen, Preparation, Characterization and drug release properties polyvinyl
alcohol and polyvinyl pyrolidone blended hydrogels, European J. Eng. App. Sci. 1
(1) (2018) 27–30.
[47] A. Tironi, M.A. Trezza, E.F. Irassar, A.N. Scian, Thermal treatment of kaolin: effect
on the pozzolanic activity, Procedia Mater. Sci. 1 (2012) 343–350, https://doi.org/
10.1016/j.mspro.2012.06.046.
[48] A. Nmiri, O. Yazoghlı-Marzouk, M. Duc, N. Hamdi, E. Srasra, Temperature effect on
mechanical and physical proprieties of Na or K alkaline silicate activated
metakaolin-based geopolymers, Ital. J. Eng. Geol. Environ. 1 (2016) 5–15, https://
doi.org/10.4408/IJEGE.2016-01.O-01.
[49] D. Panias, I.P. Giannopoulou, T. Perraki, Effect of synthesis parameters on the
mechanical properties of fly ash-based geopolymers, Colloids Surf. A Physicochem.
Eng. 301 (2007) 246–254, https://doi.org/10.1016/j.colsurfa.2006.12.064.
[50] V. Prajaputra, Z. Abidin, Widiatmaka, D.T. Suryaningtyas, H. Rizal,
Characterization of Na-P1 zeolite synthesized from pumice as low-cost materials
and its ability for methylene blue adsorption, IOP Conf. Ser. Earth Environ. Sci. 399
(2019), 012014, https://doi.org/10.1088/1755-1315/399/1/012014.
[51] M.A. Longhi, E.D. Rodríguez, B. Walkley, Z. Zhang, A.P. Kirchheim, Metakaolin-
based geopolymers: relation between formulation, physicochemical properties and
efflorescence formation, Compos. B Eng. 182 (2020) 107671, https://doi.org/
10.1016/j.compositesb.2019.107671.
[52] R.K. Chouhan, M. Mudgal, A. Bisarya, A.K. Srivastava, Rice-husk-based
superplasticizer to increase performance of fly ash geopolymer concrete, Emerg.
Mater. Res. 7 (3) (2018) 169–177, https://doi.org/10.1680/jemmr.18.00035.
[53] T. Bakharev, Geopolymeric materials prepared using class F fly ash and elevated
temperature curing, Cement Concr. Res. 35 (2005) 1224–1232, https://doi.org/
10.1016/j.cemconres.2004.06.031.