Ceramics International 48 (2022) 12932–12944

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

Mechanical and microstructural characteristics of geopolymer mortars at

high temperatures produced with ceramic sanitaryware waste
Zahide Bayer Öztürk a, *, İsmail İsa Atabey b
a
Nevsehir Haci Bektas Veli University, Department of Metallurgy and Materials Engineering, 50300, Nevsehir, Turkey
b
Nevsehir Haci Bektas Veli University, Department of Civil Engineering, 50300, Nevsehir, Turkey

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

Keywords: Excessive amounts of solid wastes are generated by the ceramic sanitaryware sector in the world. Recycling
Ceramic sanitaryware waste ceramic wastes is one of the crucial solutions to ensure their elimination. This experimental study investigates the
Geopolymer mechanical and microstructural characteristics of geopolymer mortars with recycled ceramic sanitaryware waste
Mechanical properties
powder (CSW) exposed to high temperatures. The geopolymer mixtures are produced using CSW with four
High temperature
Microstructure
different molarity (10, 12, 14, and 16 M) of NaOH as alkali-activator and two water/binder ratios (0.45 and
0.50). The investigated properties of the CSW-based Mortars (CSW-M) are the flowability, unit weight, apparent
porosity, flexural strength, compressive strength, phase, and microstructure utilizing X-ray diffractometry (XRD),
and scanning electron microscopy (SEM/EDS). The increase in NaOH concentration is observed to improve the
flow workability of CSW-M and reduce the apparent porosity and water absorption of specimens. Mechanical test
results indicate that strength values of CSW-M increase with increasing NaOH molarity. The highest strength is
obtained on the CSW-M made with 16 M NaOH and 0.45 w/b ratio. The crystalline phases are determined to be
mullite, quartz and albite derived from ceramic sanitaryware waste. Additionally, zeolite is formed by the sec­
ondary reaction product after elevated temperatures. Performance analysis results reveal that using ceramic
sanitaryware waste is a strong alternative material as a binder to produce geopolymer mortars and contributes to
the elimination of the waste.

1. Introduction or industrial wastes like fly ash, slag, ceramic wastes, and alkali acti­
vator solutions such as NaOH, Na2SiO3 [9,10]. Alkaline solutions form
Portland cement, which is a widely used binder material in concrete the structure of 3-dimensional polymeric chains of Si–O–Al [2].
technology, constitutes approximately 1.5 billion tons of CO2 emissions Although the production of geopolymer mortars with conventional
per year and 36% of global energy consumption [1]. To overcome a materials such as fly ash has become quite possible, it is necessary to
large amount of energy consumption and carbon gas emissions, serious make mortar production much more sustainable and economical by
environmental and economic issues, researchers have attempted to using local waste materials that can cause environmental hazards. Over
search for several alternatives instead of the utilization of ordinary the past few decades, various ceramic wastes such as ceramic tiles and
Portland cement such as geopolymer binders, zero-cement materials [2]. bricks have become a significant part of the alkali-activated mortars
During the last decades, geopolymer mortars/mixtures have been technology due to stability, toughness, high resistance to biological,
investigated as a new structural material in the sector of construction. chemical, and physical degradation factors [10,11]. Hence, these wastes
These mortars do not only enhance durability, high early strength, and occupy a large area of the landfill and create significant environmental
non-combustibility properties but also reduce the environmental sus­ problems due to being non-recyclable in the greatest proportion. Utili­
tainability and cost allowing the reuse of generated by-products like fly zation of these wastes helps to solve the ceramic sector waste problem
ash, slag, etc. [3–5]. The term “geopolymer” is generally used to describe and also, it enables to manufacture good quality construction materials
new “inorganic polymer” which is formed from a mix of an alumino­ [2,5,12]. The alternative usage of various industrial by-products, such as
silicate with alkaline solutions [6–8]. Geopolymers are produced by the red-clay ceramic powders [13] fine brick waste [14], red mud [15,16],
chemical reaction between aluminosilicate sources such as metakaolin glass wastes [17,18], ceramic tile wastes [5,11,12,19,20] as a

* Corresponding author. Phone: (+90) 384 228 10 00 Fax: (+90) 384 228 11 23
E-mail address: [email protected] (Z. Bayer Öztürk).

https://doi.org/10.1016/j.ceramint.2022.01.166
Received 10 September 2021; Received in revised form 14 December 2021; Accepted 16 January 2022
Available online 19 January 2022
0272-8842/© 2022 Elsevier Ltd and Techna Group S.r.l. All rights reserved.
Z. Bayer Öztürk and İ.İ. Atabey Ceramics International 48 (2022) 12932–12944

geopolymer precursor has been studied in several works. Nevertheless, 2. Materials and methods
the possibility of recovery of sanitaryware wastes for geopolymer mor­
tars and properties of ceramic sanitaryware waste-based geopolymer, 2.1. Materials
and analysis of the mechanic and microstructural performance of these
mortars at high temperatures is still needed to be studied. Ceramic sanitaryware waste powder (CSW) was supplied from Tur­
Ceramic sanitaryware (vitrified products) commonly used in bath­ kuaz Ceramic Factory in Kayseri, Turkey after the milling process. CSW
rooms and kitchens includes products such as bidets, lavatories, reser­ preparation process in the ceramic factory and CSW-based mortars
voirs, washbasins. The production of sanitaryware includes a series of (CSW-M) are shown in Fig. 1. The chemical analysis of ceramic sani­
stages which can be summarized as obtaining raw materials (clay, taryware was examined through X-ray fluorescence (XRF) in a Rigaku
kaolin, feldspar, quartz, etc.), forming in a plaster mold, drying, glazing, ZSX spectrometer, and is presented in Table 2. The mean particle di­
firing at controlled temperatures (1200◦ C–1290 ◦ C), and quality control ameters of milled CSW particles were d10, d50, and d90 of 3.85, 51.9,
[21]. Turkey is one of the leading countries in the production and export 278 μm, respectively, and analyzed by laser granulometry in a Master­
of ceramic sanitaryware, producing 320.000 tones with 21.3 million sizer 3000 in Fig. 2. X-ray diffraction analysis was performed to deter­
pieces and exporting 60% of them in Europe [22]. The percentage of mine the mineralogical composition of CSW powder. The pattern
products that are unsuitable for sale and thus discarded depends on showed that it consisted of quartz, albite and mullite phases (Fig. 3). The
technical standards, aesthetic properties, and product requirements. deviation from the baseline within the range of 15–30◦ (2 theta) in­
Nonetheless, 5–7% of these rejected pieces were reused as raw material dicates a noticeable amount of amorphous phase in the waste powder
by manufacturers [21]. In this respect, the evaluation of discarded [11]. The milled CSW particles were screened at 63 μm sieve and
products “ceramic sanitaryware wastes” in the various field needs to be morphology of CSW particles was investigated with scanning electron
investigated. Recently, the usage of ceramic sanitaryware wastes as a microscopy. Irregularly shaped particles, approximately 5–10 μm in
starting material for geopolymer mortars represents a novel approach size, were present in microstructure. According to SEM-EDS results, a
worldwide due to the limited of studies and a lack of standards regu­ detailed examination of two regions of the WSP was evaluated. EDS
lating the reuse of these wastes in construction materials [21]. In the Spectrum 1 contained 44.09 wt% O, 25.28 wt% Al, 28.76 wt% Si and
work by Reig et al. [23], the effect of Ca(OH)2, Portland cement, and 1.86 wt% Fe. EDS-Spectrum 2 contained 54.07 wt% O, 21.55 wt% Al,
calcium aluminate cement on the mechanical and microstructure 24.38 wt% Si in Fig. 4.
properties of alkali-activated mortar based on ceramic sanitaryware River sand obtained from the Nevşehir region in Turkey was
wastes was evaluated. In another work by Reig et al. [20] new binders employed for the manufacture of CSW-M. The specific gravity of the
were developed by the alkali activation of ceramic sanitaryware waste river sand used in the production of mortar was 2.67 g/cm3. The sieve
with Portland cement by partial replacement of ceramic wastes. Medina analysis of the river sand is given in Table 1. In the mixtures, NaOH was
et al. [21] investigated the possibility of reusing the ceramic sanitary­ used as an alkali activator by dissolving in water. The purity of NaOH
ware waste as a coarse aggregate in recycled concrete production. Cosa was almost 98%. Potable water was used in the production of CSW-M.
et al. [24] studied the partial use of fluid catalytic cracking residue and
SiO2 concentration instead of ceramic sanitaryware in alkali-activated 2.2. Methods
systems. The waste/residue combinations significantly improved me­
chanical properties under the studied conditions. Ozturk et al. [25] In this study, four CSW-M were produced for each series according to
worked on the effect of sanitaryware wastes on the development of the molarity of NaOH. The quantities of materials in the mixtures for
properties of fly ash-based geopolymer mortars. The results of me­ three cell mold in 40 × 40×160 mm size are presented in Table 3. The
chanical properties showed that the variation of ceramic sanitaryware water to binder ratios (w/b) of 0.45 and 0.50 were selected to prepare
wastes instead of fly ash improved strength development favorably. In mortar specimens. Sand/CSW ratio was taken as 3. The molar concen­
another study by Atabey and Ozturk [26], the effects of different liq­ tration of NaOH in the mixtures was determined as 10, 12, 14 and 16 M.
uid/binder ratios and molarity were investigated on the ceramic sani­ The mixes were prepared in the Hobart-type laboratory mixer. Then,
taryware waste-based alkali-activated mortars. In terms of improved fresh geopolymer mortars were placed in molds. These mortars were
strength, economic, and environmental conditions, it was determined prepared according to the TS EN 196-1 [28]. The geopolymer mortar
that the appropriate water content for geopolymer mortar production specimens placed into the molds were cured in a laboratory oven at
was w/b:0.45. According to the study by Gaibor et al. [27], ceramic 100 ◦ C for 24 h. After the heat curing time, specimens were demolded
wastes such as ceramic tiles and sanitaryware products were used in from their cast then allowed to cool down to ambient. Then, specimens
alkali-activated binders mixed with fly ash or ladle furnace slag acti­ were subjected to experimental tests. Three specimens were produced
vated with sodium silicate. Compressive strengths were achieved almost for each mortar mixture. Mixtures were encoded depending on the
20 MPa and 59 MPa after 90 days in mortars. water/binder ratio, ceramic sanitaryware waste (CSW), and NaOH
Experimental studies in the literature clearly show that ceramic molarity, respectively (e.g. 45CSW10).
wastes (especially ceramic tiles, bricks, etc.) exhibit high mechanical According to TS EN 1015-3 [29], a flow table test was conducted to
characteristics and are used as an alternative material in alkali-activated measure the flowability of fresh mortars. For each geopolymer mortar
mortars. Nevertheless, these experimental results were obtained mostly flowability, the flow diameter of fresh mortar was determined. The unit
with ceramic wastes of different ratios replaced by fly ash or slag. There weight (UW) test was applied on the geopolymer samples after 24 h from
is a lack of experimental data on the microstructural and mechanical the heat-curing. Apparent porosity (AP) and water absorption (WA) tests
characteristics of geopolymer mortars produced with CSW as the sole were conducted to measure the transport characteristics of mortars ac­
precursor. Present study mainly aims to reduce the waste amount of the cording to ASTM C642 [30]. On the hardened CSW-M, Flexural Strength
ceramic industry by using 100% CSW for geopolymer mixtures. For this (FS) tests were carried out using prismatic (40 × 40×160 mm) samples
purpose, the study aims to investigate the effect of two w/b ratios, four under 3-point loading conditions explained in TS EN 1015-11 [31]. The
molarity concentrations of NaOH as an alkali-activator and high tem­ average of the results of three CSW-M samples was determined as the
peratures on the mechanical and microstructural characteristics of CSW- flexural strength value. The Compressive Strength (CS) was identified on
M. The mechanical, microstructural and phase characteristics of the the broken pieces of the prismatic samples after the flexural strength test
CSW-M subjected to temperatures of 400 ◦ C and 800 ◦ C are studied. (TS EN 1015-11). The CS tests were performed on two fragments of each
Besides, the results of the flow table, unit weight, apparent porosity, and specimen retained after the FS tests of the unheated (only curing tem­
water absorption of CSW-M are presented. perature, at 28 days) and heated (exposure to 400 ◦ C, and 800 ◦ C tem­
peratures, at 28 days) CSW-M. The loading area and loading rate in the

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Fig. 1. Ceramic sanitaryware powder preparation process in factory and mortar production in the laboratory.

3. Results and discussions

Table 1
The sieve analysis values of sand.
3.1. Workability
Sieve diameter, mm Sieved, %

4.00 99.1 The workability results of fresh mortars are given in Table 4. The
2.00 65.1 table shows that an increase in molar concentration improved the flow
1.00 40.2
diameter of mortars. The flow diameters for the w/b:0.45 geopolymers
0.5 21.3
0.25 9.9 were measured between 103 and 115 mm while these values were be­
0.125 3.7 tween 158 and 192 mm in the mixtures with w/b:0.50. By increasing
0.063 0.9 NaOH molarity from 10 to 16, the flow diameter increased by 12% for
w/b:0.45, 22% for w/b:0.50. In general, the workability of the fresh
mixes increased with the increase in the w/b. An increase of 5% in water
CS tests were 40 × 40 mm2 and 500 N/s, respectively. An average of six
content contributed significantly to workability. It is known that an
broken pieces were used for compressive strength values. A
increase in the ratio of water/binder in the mixture causes to increase
high-temperature test of mortars was carried out for two different
workability [2,32].
temperatures as 400 ◦ C and 800 ◦ C. An electric furnace was used for the
An increase in water amount of mixture reduces the molarity of the
high-temperature test. The furnace’s temperature was increased by
alkali activator, resulting in a reduction in viscosity of composition and a
5 ◦ C/min and kept at the target temperature degree for 60 min. Then, the
slow rate of geopolymerization improved workability [33]. In addition,
furnace was turned off, and the samples were left to cool down slowly for
high sodium concentration improved workability. While NaOH con­
24 h before testing. After high-temperature exposure, compressive and
centration increased in mortars from 10 M to 16 M, workability values
flexural strengths of specimens were measured and compared with
increased in CSW-based fresh mortars. The flow values of the CSW-M
values prior to the heating. The CSW-M unexposed to high temperature
increased from 103 to 158 mm, 109–170 mm, 110–180 mm, and
(exposed to only curing temperature) and subjected to temperatures of
115–192 mm with increasing w/b ratio at the molarity of 10, 12, 14, and
400 ◦ C and 800 ◦ C were selected for the microstructure and phase an­
16 M, respectively. In a previous work, Durak et al. revealed that as
alyses. The samples were evaluated in terms of phase and microstruc­
sodium concentration increased in the mortar, workability also
tural analyses to determine how CSW and variation of molar
increased [34]. While sodium molarity increased in the mortar from 8 to
concentration were chemically affected.
10% and 12%; flow diameter improvements were observed as

Table 2
The chemical composition of ceramic sanitaryware waste.
SiO2 Al2O3 K2O Fe2O3 CaO TiO2 ZrO2 Na2O MgO ZnO P2O5 L.O.I

66.32 27.86 1.56 1.25 1.07 0.59 0.51 0.37 0.16 0.10 0.05 0.10

L.O.I: loss on ignition.

Fig. 2. Particle size distribution of ceramic sanitaryware waste.

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the NaOH molarity, which has a higher density compared to water,

increased the UW of the NaOH solutions [35]. A similar tendency in the
UW of the CSW-M with the NaOH concentration was emphasized for the
raw perlite [36], metakaolin [37], bottom ash-based [38] geopolymer
mortars.

3.3. Apparent porosity and water absorption

The apparent porosity (AP) and water absorption (WA) values of

CSW-M are illustrated in Fig. 5. A decrease in WA and AP was observed
with increased NaOH molarity from 10 M to 16 M. For w/b:0.45 geo­
polymers mixtures, WA values were calculated to be between 11.7% and
17.6% while AP values were between 6.1% and 9.1%. Similarly, for w/
b:0.50 geopolymer mortars, WA values were calculated between 18.7%
and 21.6% while AP values were between 9.6% and 11.3%. The increase
in molarity of NaOH can remarkably decrease the WA ratio as well as the
AP of CSW-M.
Fig. 3. XRD patterns of ceramic sanitaryware waste (albite: (Na,Ca(Si,Al)4O8,
mullite: Al4.44Si1.56O9.78, quartz: SiO2)
Table 3
Mixture proportions of geopolymer mortars.
approximately 12% and 20% compared with 8% Na concentration.
w/b Codes of CSW Water Sand Molarity NaOH
Mixtures (CSW- (g) (g) (g) (M) (g)
3.2. Unit weight M)

0.45 45CSW10 450 202.5 1350 10 81.0

The unit weight (UW) of hardened CSW-M is shown in Table 5. UWs 45CSW12 450 202.5 1350 12 97.2
of CSW-M were between 1.92 and 1.99 g/cm3 for w/b:0.45. In the same 45CSW14 450 202.5 1350 14 113.4
manner, UWs of the w/b:0.50 samples were between 2.00 and 2.10 g/ 45CSW16 450 202.5 1350 16 129.6
0.50 50CSW10 450 225.0 1350 10 90.0
cm3. The minimum UW was obtained as 1.92 g/cm3 on the 45CSW10 50CSW12 450 225.0 1350 12 108.0
mortars, and the maximum UW was obtained as 2.10 g/cm3 on the 50CSW14 450 225.0 1350 14 126.0
50CSW16 mortars. The UW values of the CSW-M slightly increased by 50CSW16 450 225.0 1350 16 144.0
incrementing NaOH concentration. The reason for this increment is that

Fig. 4. SEM-EDS analysis of CSW.

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Table 4 50CSW10 mortars while the highest FS values were seen in the
Flow diameter and unit weight of hardened samples. 45CSW16 mortars. The highest FS was 6.4 MPa obtained from mixture
w/b Mixtures (CSW-M) Flow Diameter, mm 45CSW16 mortars. Fig. 6 also shows that an increase in NaOH concen­
tration increases FS strength for all w/b. On the other hand, while
0.45 45CSW10 103
45CSW12 109 molarity is higher than 14 M, an increase in the concentration did not
45CSW14 110 significantly contribute to FS for w/b:0.45 mortars. The FS of the w/
45CSW16 115 b:0.45 containing mortars increased by 7% with the increase of molarity
0.50 50CSW10 158 from 14 M to 16 M concentrations. On the other hand, when the FS of the
50CSW12 170
50CSW14 180
samples increased from 10 M to 12 M concentration an increment was by
50CSW16 192 56%. High concentration (16 M NaOH) did not clearly affect the FS of w/
b:0.45 geopolymer mortars unlike w/b:0.50. The CSW-M in the series of
w/b:0.50, with molarity increased from 10 M to 14 M, FS increased
approximately by 86% and from 14 M to 16 M, FS increased by 29%.
Table 5
Flow diameter and unit weight of hardened samples. After exposure to 400 ◦ C and 800 ◦ C, the 50CSW10 exhibited the
lowest FS of 1.6 and 1.9 MPa, respectively. The FS of CSWs coded with
w/b Mixtures (CSW-M) Unit Weight (UW), g/cm3
45CSW10, 45CSW12, 45CSW14, and 45CSW16 were 2.2, 2.6, 2.8 and
0.45 45CSW10 1.92 3.6 MPa after exposure to 400 ◦ C, respectively. The FS values of CSW-M
45CSW12 1.94
coded with 50CSW10, 50CSW12, 50CSW14 and 50CSW16 were 1.9, 2.8,
45CSW14 1.96
45CSW16 1.99 3.2, and 3.6 MPa after exposure to 400 ◦ C, respectively. FS loss was less
0.50 50CSW10 2.00 at w/b:050. The FS values of CSW-M decreased gradually with the in­
50CSW12 2.05 crease in temperature. The FS values of CSW-M coded with 45CSW10,
50CSW14 2.07 45CSW12, 45CSW14 and 45CSW16 were 1.8, 2.2, 2.3 and 3.0 MPa after
50CSW16 2.10
exposure to 800 ◦ C, respectively. After exposure to 800 ◦ C, the FS of
CSW-M coded with 50CSW10, 50CSW12, 50CSW14 and 50CSW16 were
The reduction in AP could be attributed to the higher density, which 1.6, 2.2, 2.7 and 3.1 MPa, respectively. At 400 ◦ C, the FS values of
increased the WA of the specimen. Increased molarity of NaOH leads to mortars for w/b:0.45 and w/b:0.50 were slightly higher than the ones
rise in Na2O content and increasing of solution viscosity improved more exposed to 800 ◦ C. The FS values of the CSW-M continuously decreased
homogeneous and denser surface with less porosities as reported in together with increasing temperature. One of the major reasons for this
microstructure analysis [39]. A higher NaOH molarity had a better reduction in the FS is that the interface transition region was influenced
ability to dissolve CSW particles, resulting in a better geopolymeric re­ by high temperature and cracks occurred in this zone as a result of this
action. The increase of the molarity in the CSW-M resulted in the in­ effect [41].
crease in leaching of Si and Al from the CSW particles to the solutions.
This resulted in a dense and strong geopolymer matrix which decreased 3.5. Compressive strength
the WA and AP of the samples [40].
Compressive strength (CS) of CSW-M activated by NaOH are pre­
3.4. Flexural strength sented in Fig. 7. The CS values of the 45CSW were determined as 22.3,
30.4, 34.1, and 36.0 at the molarity of 10, 12, 14, and 16 M, respectively.
The flexural strength (FS) values of samples before and after expo­ Besides, the CS values of CSW-M coded with 50CSW10, 50CSW12,
sure to 400 ◦ C and 800 ◦ C are presented in Fig. 6. The FS values of the 50CSW14 and 50CSW16 were 16.7, 22.5, 24.7 and 30.4 MPa, respec­
CSW-M improved significantly as the molarity increased from 10 M to tively. As shown in Fig. 7, the highest CS was 36.0 MPa obtained from a
16 M, and in particular from 10 M to 12 M. The FS values of the CSW-M mixture of 45CSW16. The CS values of the CSW-M with increasing
changed between 3.6 and 6.4 MPa for the w/b:0.45, and 2.2–5.3 MPa for molarity of NaOH from 10 M to 16 M increased significantly, especially
the w/b:0.50. In all the CSW-M, the lowest FS values were seen in the from 10 M to 12 M for w/b:0.45. This can be explained as the higher

Fig. 5. Water absorption and apparent porosity values of mortars.

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Fig. 6. Flexural strength values of mortars.

Fig. 7. Compressive strength values of mortars.

molarity has better capability to dissolve CSW powders and results in curing temperatures affect the strength value. In Atabey et al. [45], the
better alkali reaction [42,43]. With regard to the influence of the w/b highest strength value obtained curing temperature at 100 ◦ C.
ratio, decreasing the value of w/b enhanced the CS, which reached its The CS of the CSW-M was obtained at different ratios with the effect
maximum value at w/b:0.45. The decrease in apparent porosity (AP) of temperature. After being subjected to 400 ◦ C, and 800 ◦ C, the CSW-M
with increasing NaOH molarity was in parallel with an increase in exhibited the lowest residual CS of 70% and 39%, respectively. After
strength at every two alkaline solution-to-binder ratios. For instance, at being subjected to 400 ◦ C, the residual CS of CSW-M coded with
constant w/b of 0.45, AP decreased from 9.1% to 6.1% for the molarity 45CSW10, 45CSW12, 45CSW14, and 45CSW16 were 80%, 70%, 70%
increase from 10 M to 16 M. In parallel with these results, the CS and 70%, respectively. The residual CS values in the mixture series of w/
increased from 22.3 MPa to 36.0 MPa for the molarity increase from 10 b:0.50 were higher than the w/b:0.45. The residual CS values of CSW-M
M to 16 M. A similar trend was found for the other w/b ratio. In general, coded with 50CSW10, 50CSW12, 50CSW14, and 50CSW16 were 92%,
similar to cement mortar, a lower amount of water phase provides more 76%, 88% and 81% after exposure to 400 ◦ C. In the CSW-M, the lowest
efficient hardening but a sufficient amount of activator is required to residual CS value of 39% was observed on the mixture coded with
achieve a complete geopolymeric reaction. Nevertheless, the increase in 45CSW14. Rashad and Khalil [46] stated a decrease in the CS of
water content increased the porosity. Thus, a reduction in CS was alkali-activated pastes after exposure to 400 ◦ C and 800 ◦ C. Wang et al.
observed at w/b of 0.50, which could be related to the high-water [47] emphasized a reduction in the CS of alkali-activated pastes after
amount [3]. The variation in the CS values of the CSW-M with exposure to 200 ◦ C, 500 ◦ C, and 800 ◦ C.
increasing molarity was similar to the FS values. When the NaOH As shown in Fig. 8, all the CSP-M exhibit CS losses after exposure to
molarity was high, the dissolution of Si4+ and Al3+ ions from CSW 400 ◦ C, and 800◦ . It was observed that compressive strength loss was
increased and the formation of sodium aluminosilicate was enhanced higher as the level of temperature got higher. 45CSW14 and 45CSW16
leading to an increase in FS and CS [44]. Besides, it was investigated that mortars exhibited the highest strength losses in similar ways. These

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experimental results indicated that the CS values of CSW-M containing part of crystal phases (albite and quartz) into amorphous phase or
excess sodium hydroxide (45CSW14 and 45CSW16) were much more semi-crystal geopolymer gel [5,56]. Apparently, the concentration of
affected by elevated temperature than the other CSW-M because of the molarity increased as the intensity of the amorphous hump slightly
thermal expansion of free Na⁺ ions dissolved from the sodium hydroxide increased due to higher sodium content.
[48]. Additionally, the trends in the FS tests are very similar to the ones
in the CS tests. The FS value of the CSW-M increased by 56% with the 3.7. SEM and EDS analyses
increase of NaOH concentration from 10 M to 12 M, for 16 M concen­
tration the increment was by 78% for w/b = 0.45. For CS, these values A secondary electron (SE) mode was used to observe changes in the
are 53% and 61%, respectively. The CS and FS reductions after high microstructure of selected samples. The samples which have the opti­
temperature are also similar. For example, FS and CS reduction of 53% mum solution/binder ratio (i.e. w/b = 0.45) were selected for micro­
and 60% was observed on the mixture coded with 45CSW16 from 100 ◦ C structure analysis. The strength values (FS and CS) were influenced by
to 800 ◦ C, respectively. increasing NaOH molarity. Therefore, samples prepared with 10 M and
16 M NaOH solutions were analyzed to evaluate the effect of molar
3.6. XRD analysis concentration. The images shown in Fig. 11(a–f) indicate the amount
and size of mullite, albite, quartz crystals. As can be seen from the
The phases of CSW-M exposure to different temperatures are seen in microstructure images of the 45CSW10-100 ◦ C and 45CSW16-100 ◦ C
Figs. 9 and 10 for the 45CSW10 and 45CSW16, respectively. The major samples in Fig. 11(a), (d) small-sized albite crystals of approximately
crystalline phases were identified as mullite, quartz, and albite derived 0.4 μm, 1–2 μm sized and highly homogeneous distribution with mullite
from ceramic sanitaryware waste. Zeolite as a minor constituent in the crystals occurred in these samples. Furthermore, partially reacted and
experiment, as observed by Huseien et al. [4], was formed by the sec­ unreacted particles (mullite and albite) originate from CSW have in the
ondary reaction product after high temperatures. After exposure to microstructure of the 45CSW16-100 ◦ C samples leading to a homoge­
400 ◦ C and 800 ◦ C, the peak of quartz was reduced wherein the peaks of neous distribution of crystals and compaction. For the above-mentioned
mullite, albite, and zeolite became progressively stronger. At these reasons, the CS values of 45CSW16 increased.
temperatures, quartz and albite started to dissolve partially. Therefore, On the other hand, both relatively denser geopolymer matrix and the
the zeolite (NaCaAl3Si3O12) peak intensity at 800 ◦ C exhibited an in­ high size of needled mullite crystals, porosities can be seen in Fig. 11 b-c
crease compared to that of the samples at 100 ◦ C and 400 ◦ C. Zeolites are and e-f after exposure to 400 ◦ C and 800 ◦ C. This result demonstrates
hydrated aluminosilicates of alkaline and alkaline earth metals forming that quartz and albite crystals dissolved and a more cohesive geo­
a group of minerals which contains intracrystalline channels or inter­ polymer matrix was observed. But the porosities were determined to
connected voids based on SiO4 and AlO4 tetrahedrons [49]. The litera­ increase with increasing temperatures and sodium content due to NaOH
ture includes certain studies concerning zeolitic crystal-based composite molar concentration and albite dissolution. Homogeneous structures of
materials in geopolymeric matrices, that the studies mainly describes alkali-activated mortars were transformed to the less compact form with
two processing routes: (a) incorporating commercial zeolites during a visible network of micro-cracks and large pores which are more pro­
alkaline activation [50,51], or (b) promoting solid-state reactions where nounced with the high temperatures [4]. This explains the decrease in
part of the amorphous geopolymer gel is converted to zeolitic crystals CS at 400 ◦ C and 800 ◦ C. The size of the needled mullite affected by the
during hydrothermal curing [52–54]. This can occur because higher temperature increased. Hence, the porosity formation with poor
temperatures increase the internal pressure in the samples favoring the microstructure increased. This particular issue also negatively affected
formation of these crystals [ 53]. The broad and diffused background the mechanical properties, where the CS decreased from 22.3 to 36.0
peak in the samples with 16 M concentrations was displaced toward a (45CSW10 and 45CSW16 at 100 ◦ C) to 11.9–14.3 MPa by replacing
relatively amorphous structure in Fig. 10. Hwang et al. [55] stated that a 100 ◦ C with 400 ◦ C and 800 ◦ C.
reduction in the peaks of quartz and an increase of molar concentration According to the SEM-EDS results of the 45CSW10-100, while albite
were sites of alkali reactions that augment geopolymeric reaction into crystal was contained 36.6 wt% O, 20.6 wt% Na, 16.82 wt% Si, 12.77 wt
the gel matrix. This state has created an advantage in improving the CS % Al, 10.58 wt%C and 1.08 wt% Fe in Fig. 12(a), mullite regions con­
and porosity of the 45CSW16 series. The intensity of albite peaks tained 46.59 wt% O, 15.08 wt%Si, 9.74 wt% Al, 12.71 wt%Na, 15.87 wt
showed a small reduction in 400 ◦ C and 800 ◦ C compared with 100 ◦ C. % C in Fig. 12(b). Albite containing phase region involved 47.83 wt% O,
This illustrates that high temperature was able to dissolve and transform 20.5 wt%Si, 15.79 wt%Na, 15.1 wt% Al, mullite regions contained
49.89 wt%O, 20.41 wt%Si, 16.14 wt% Al, 13.55 wt%Na for 45CSW10-
400 ◦ C in Fig. 13. On the other hand, albite regions were detected as
42.43 wt% O, 27.89 wt% Si, 12.3 wt% Al, 8.78 wt%Na, 5.01 wt% K and
3.59 wt% Fe in 45CSW10-800 (Fig. 12). 45CSW16 series samples have
the highest amount of NaOH concentration and the highest amount of
Na-containing phases added into the geopolymer mortars. For this
reason, the microstructure of these samples is different from other
compositions which contain a higher amount of Na. This demonstrates
that increasing the molarity of NaOH solution was able to dissolve and
transform part of these crystal phases (mullite and albite) and resulted in
better activation of CSW [56,57]. For 45CSW16-100 ◦ C, the
albite-containing region contained 45.99 wt% O, 19.97 wt% Na, 19.02
wt% Si and 13.27 wt% Al, mullite regions contained 46.88 wt% O,
21.32 wt%Si, 7 wt% Al, 17.35 wt%Na, 4.48 wt%C (Fig. 14). For
45CSW16-400 ◦ C, albite containing region contained 43.54 wt% O,
16.58 wt% Na, 24.92 wt% Si and 12.89 wt% Al, mullite regions con­
tained 46.12 wt% O, 19.42 wt%Si, 11.52 wt% Al and 22.18 wt%Na
(Fig. 15). The higher size of mullite and porosities in the microstructures
of 45CSW16 were obtained at high temperature (800 ◦ C) compared with
Fig. 8. Residual compressive strength results of mortars exposed to elevated other samples. This explains the lower compressive strength at 800 ◦ C.
temperature. For 45CSW16-800 ◦ C, albite containing dense region contains 34.79 wt

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Fig. 9. XRD analysis results of 45CSW10 before and after exposure to elevated temperatures (quartz: SiO2, mullite: Al6Si2O13, Albite: Al2O3Na2O6SiO2, Zeolite:
NaCaAl3Si3O12).

Fig. 10. XRD analysis results of 45CSW16 before and after exposure to elevated temperatures (quartz: SiO2, mullite: Al6Si2O13, Albite: Al2O3Na2O6SiO2, Zeolite:
NaCaAl3Si3O12).

% O, 13.62 wt% Na, 44.35 wt% Si, 4.27 wt% Al, and 2.97 wt%Ca, could be caused by a higher degree of dissolution of aluminosilicates and
mullite regions contain 39.21 wt% O, 26.6 wt%Si, 14.36 wt% Al, 1.58 wt greater formation of geopolymeric product in the 45CSW16 series due to
%K and 16.75 wt%Na (Fig. 16). The literature also implies that an an increment in NaOH molar concentration [56]. When the temperature
increment in CSW imposes negative effects on C-A-S-H gels formulation increased to 400 ◦ C and 800 ◦ C, this dissolution can be attributed to
and produces more partially reacted gel such as mullite and non-reacted needle mullite and zeolite crystallizing and growing in the geopolymeric
particles including quartz [19,58]. On the other hand, high Si, Na, Al gel. Furthermore, the main high size of mullite and zeolite crystallized
contents in mixtures indicate the formation of sodium aluminosilicate structure of samples at 800 ◦ C might lead to heterogeneous micro­
hydrate (N-A-S-H) gels as the main reaction product during geo­ structure and some flaws such as microcracks and porosities which
polymeric reaction [56]. The CSW amount was stable as 450 gr in mortar negatively affect the CS [5]. De Silva stated that the variation in geo­
mixtures of this work. The microstructures of 45CSW16 series samples polymer matrix microstructure into crystalline zeolites may have
were relatively more cohesive and denser geopolymer matrix (Fig.9 d-e-f created negative influences on mechanical strength in their study [59].
and Figs. 15–17) compared to 45CSW10 series samples (Fig. 11 a-b-c). The loss of strength at elevated temperatures is found to be linked to the
This demonstrates that the balanced SiO2/Al2O3 and Na2O/SiO2 ratios increase of loss of N-A-S-H gels and surface energy of gel coming into

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Fig. 11. SEM images of 45CSW16 showing the effect of being subjected to temperatures at a)100 ◦ C, b)400 ◦ C, c)800 ◦ C (M: mullite, A: albite; Q: quartz, P: porosity,
D: dense region).

Fig. 12. EDS spectra and spot/square analysis of sample 45CSW10-100 ◦ C (a)mullite regions, (b)albite.

existence due to the loss of water from the surface and partially dis­ experimental results and analysis, the following conclusions can be
solved mullite and quartz crystals, new-formed zeolites. The appearance drawn:
of dispersed smaller pores in the structure caused the loss of strength
[60]. ● The augment of NaOH molarity resulted in improved workability of
CSW-M. Nevertheless, the decrease of the ratio of water/binder in
4. Conclusions the mixture causes reduced workability due to a reduced water
amount of alkali solution. The unit weight of CSW-M prepared with
This study reveals the waste disposal potential of ceramic sanitary­ the ratio of w/b:0.45 was found to be less when compared to samples
ware waste-based geopolymers with suitable mechanical and micro­ prepared with the ratio of w/b:0.50.
structure performance as construction materials. Based on the

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Z. Bayer Öztürk and İ.İ. Atabey Ceramics International 48 (2022) 12932–12944

Fig. 13. EDS spectra and spot/square analysis of sample 45CSW10-400 ◦ C (a)mullite regions, (b)albite.

Fig. 14. EDS spectra and spot/square analysis of sample 45CSW10-800 ◦ C (albite region).

Fig. 15. EDS spectra and spot/square analysis of sample 45CSW16-100 ◦ C (a) mullite regions, (b) albite.

● A decrease in WA and AP was observed with increased NaOH ● The crystalline phases identified as mullite, quartz, and albite were
molarity from 10 M to 16 M whilst these values were increased in w/ derived from ceramic sanitaryware waste. Besides, zeolite was
b: 0.50 compared to w/b:0.45. formed by the secondary reaction product after elevated tempera­
● The strengths (CS-FS) of CSW-M increased by incrementing NaOH tures (400 ◦ C and 800 ◦ C). The intensity of quartz and albite peaks
concentration. Samples produced with 16 M NaOH reached the showed a small reduction in 400 ◦ C and 800 ◦ C compared with
highest strengths. Nevertheless, the favorable influence of molarity 100 ◦ C. This demonstrates that the crystal phases (albite and quartz)
on strengths diminished with the increase in elevated temperatures were dissolved into a semi-crystalline geopolymer.
(at 400 ◦ C and 800 ◦ C) and in w/b: 0.50. ● Small albite crystals of approximately 0.4 μm, 1–2 μm sized and
● An increment of NaOH concentration enhanced the dissolution of highly homogeneous distribution with mullite crystals occurred in
quartz, albite and improved the compressive strengths and micro­ the SEM images of the 45CSW10-100 ◦ C and 45CSW16-100 ◦ C
structure of CSW-M. samples. Furthermore, partially reacted and unreacted particles

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Z. Bayer Öztürk and İ.İ. Atabey Ceramics International 48 (2022) 12932–12944

Fig. 16. EDS spectra and spot/square analysis of sample 45CSW16-400 ◦ C (a) mullite regions, (b) albite.

Fig. 17. EDS spectra and spot/square analysis of sample 45CSW16-800 ◦ C (a) mullite regions, (b) dense region.

(mullite and albite) originated from CSW particles can be seen in the Acknowledgement
microstructure of the 45CSW10-100 ◦ C and 45CSW16-100 ◦ C sam­
ples leading to a homogeneous distribution of crystals thus, The authors would like to thank Turkuaz Ceramic (Kayseri/Turkey)
increasing the compressive strengths. Nonetheless, both relatively for their support with waste materials.
denser geopolymer matrix and high size of needled mullite crystals,
porosities have been seen in samples after exposure to 400 ◦ C and References
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