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Effects of Waste Ceramic As Cement and Fine Aggregate On Durability Performance of Sustainable Mortar

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Arabian Journal for Science and Engineering

https://doi.org/10.1007/s13369-019-04198-7

RESEARCH ARTICLE - CIVIL ENGINEERING

Effects of Waste Ceramic as Cement and Fine Aggregate on Durability


Performance of Sustainable Mortar
Hossein Mohammadhosseini1 · Nor Hasanah Abdul Shukor Lim1 · Mahmood Md. Tahir1 · Rayed Alyousef2 ·
Mostafa Samadi1 · Hisham Alabduljabbar2 · Abdeliazim Mustafa Mohamed2

Received: 13 January 2019 / Accepted: 11 September 2019


© King Fahd University of Petroleum & Minerals 2019

Abstract
In the last 3 decades, the attention in consuming substitute materials such as solid wastes in construction has grown continu-
ously. An extensive amount of waste ceramic is being generated all around the world. These wastes are mostly sent to the
landfill without considering recycling option. Such waste ceramic in the powder and fine particle forms has good potential
in the infrastructure industry. In this study, the strength and durability properties of a mortar comprising ceramic waste pow-
der as supplementary cementing material and ceramic particles were investigated. Properties studied include workability,
compressive and tensile strengths, chloride and sulfate resistance. The effect of waste ceramic was also assessed by using
scanning electron microscopy and X-ray diffraction analysis. It was observed that the utilization of waste ceramic in both
forms of binder and fine aggregate significantly improved the compressive and splitting tensile strengths and higher resist-
ance against chloride and sulfate attacks. The microstructure of the mortar was further enhanced by replacing ceramic waste
powder and fine aggregates. It, therefore, caused in the higher crystalline formation and reduction in porosity and cracks in
addition to eliminating the spalling behavior of mortar specimens exposed to chloride and sulfate attacks.

Keywords  Ceramic waste · Mortar · Compressive strength · Chloride and sulfate attacks · Sustainability

1 Introduction recycle these ceramic wastes and, therefore, send to land-


fill. Consequently, there is a need for ceramic industries to
In 2012, around 12 billion m2 of various types of ceramic find an alternative way for ceramic waste disposal [4, 5]. In
tiles were produced all around the world [1]. Ceramic tiles this regard, Torgal and Jalali [6] pointed out that the use of
are manufactured by firing clay, feldspar and quartz at high ceramic waste in the sustainable construction materials such
temperatures. The total production of Malaysia in the same as mortar and concrete aids in saving the energy and cost in
year was approximately 92 million m2 [2], and the produc- construction, decreasing the ecological impacts and reduc-
tion rate is growing by 2.3% yearly It was estimated that ing the consumption of raw materials. Therefore, the idea of
as much as 10–30% of the total ceramic production goes sustainability and green production persuades the consump-
to waste [3]. The waste products from the ceramic indus- tion of various sorts of domestic and industrial wastes to use
tries are durable and highly resistant to chemical and physi- as supplementary cementing materials, aggregates or even
cal degradation forces. However, there is no technology to admixtures. It, therefore, leads to eco-friendly construction
by reducing the cost of construction associated with dispos-
ing of waste materials [7, 8].
* Hossein Mohammadhosseini Thus far and to the authors’ best knowledge, there is no
hofa2018@yahoo.com; mhossein@utm.my literature on the combined effects of the ceramic powder
1
Institute for Smart Infrastructure and Innovative and fine ceramic aggregates on the durability performance
Construction (ISIIC), School of Civil Engineering, Faculty of mortar. However, a great deal of attempts has been made,
of Engineering, Universiti Teknologi Malaysia (UTM), and various practices have been used to utilize waste mate-
81310 Skudai, Johor, Malaysia rials such as ceramic waste as partial cement replacement
2
Department of Civil Engineering, College of Engineering, or fine aggregates to enhance the performance of concrete
Prince Sattam Bin Abdulaziz University, Alkharj 11942, and mortar. Medina et al. [9] and Subaşı et al. [10] reported
Saudi Arabia

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Arabian Journal for Science and Engineering

that the concrete incorporating fine ceramic aggregates up to products of cement, such as calcium aluminate, are mostly
50% as natural aggregates could address the higher strength affected. Additional reactions among the formed gypsum
and durability performance of concrete. Besides, Suzuki and the cement particles, for example, calcium aluminate,
et al. [4] stated that the using of waste ceramic up to 40% as can similarly form the additional amount of ettringite, then
coarse aggregates in high-performance concrete revealed a initiating more cracks and results in the reduction of strength
significant reduction in autogenous shrinkage. Meanwhile, and lower durability performance [24].
Binici [11] studied the long-term compressive strength There are various techniques to enhance the durability
of concrete with 100% replacement of fine aggregates by characteristics of concrete specimens. For example, having
waste fine ceramic particles and found only 10% reduction a solid and dense microstructure by providing well-graded
in the strength. Senthamarai et al. [12] and Rashid et al. [13] particles size distribution for minimizing the entrance of
also investigated the effects of the ceramic waste powder harsh materials into the specimens improves the strength
as cement replacement and found that the waste ceramic as well as present better durability performance in concrete
powder is potential to be used as supplementary cementing through the inclusion of admixtures [25]. This method can
materials with adequate strength and durability performance significantly improve the durability and strength of concrete
in concrete. and mortar exposed to aggressive environments, as stated
Parghi and Alam [14] examined the physical and mechan- by Bolat et al. [26] and Higashiyama et al. [27]. Since the
ical properties of the cementitious composites comprising utilization of supplementary cementing materials has been
recycled glass powder (RGP), and they described that using established to develop the mechanical and durability prop-
RGP leads to the higher compressive strength due to higher erties of concrete and mortar, it paves the way for the uti-
silica and aluminum content as well as an excellent poz- lization of waste ceramic in the form of powder as cement
zolanic reaction. In their studies, Halicka et al. [15] and replacement and fine particles to enhance the long-term
Medina et al. [16] stated that the tensile strength of mortar performance of mortar under sulfate and chloride attacks.
increased as the percentage of ceramic waste used to sub- Nevertheless, studies on the application of waste ceramic in
stitute natural aggregate rose. They also found that with a mortar under aggressive environments are limited. Due to
substitution percentage of 25% ceramic fine aggregates, the the local availability of waste ceramic in Malaysia as well as
tensile strength increased by about 12% as compared to the the adequate properties of waste ceramic, extensive research
reference concrete. work was conducted to assess the potential benefits of waste
One of the most prevalent and common forms of chemical ceramic in the manufacture of sustainable and durable mor-
attacks is the action of sulfates on the mortar and concrete tar. The use of ceramic wastes would not only aid in getting
components. Sulfates are commonly found in groundwater them applied in a mortar and other construction materials,
when it occurs in sulfate-bearing formations with soils rich but instantaneously, it helps in reducing landfill area and
in sulfate minerals. Besides, seawater also has sulfate as a conserving the environment from possible pollution impacts.
major component. Concrete and mortar are susceptible to
spalling and cracking when exposed to chemicals such as
chloride and sulfate, which are essentially inescapable and 2 Materials and Test Method
frequently expected in aggressive environments [17]. The
presence of pores and cracks in concrete and mortar is the 2.1 Materials
significant problems to reduce the durability performance
[18–20]. The nature of the sulfate solution is significant, as Ordinary Portland cement (OPC) was used in this study.
the influence of other chemicals can affect the mechanism of Waste ceramic particles were collected from the local tile
the reaction. Concrete and mortar suffer degradation under industries, which are broken pieces of tiles. The waste
the impact of such aggressive environments, owing to chem- ceramic particles then were dried in an oven at a tempera-
ical processes relating to the exchange of ions. These chemi- ture of 110 °C for 24 h. Further, the bigger particles were
cals attack the hydration products of cement such as C–S–H crushed in smaller pieces with different size and shapes.
structure as well as the formation of gypsum and ettringite. The fine ceramic particles were then sieved through the
The development of these additional products results in vari- standard sieves specified by ASTM C33-13 to remove
ations of the microstructure of matrix and therefore leading large particles in order to range between the standard lim-
to the deterioration of the concrete [21]. its for fine aggregates. The fineness modulus of the natural
In regard to the said matters, Chen et al. [22] and Sotiri- river sand and fine ceramic aggregates was found as 2.64
adis et al. [23] studied the effects of the sulfate attacks on the and 2.98, respectively. In order to use the waste ceramic
concrete components. Based on their findings, sulfate attack as a cement replacement, the very fine particles were then
in concrete or mortar leads to the development of exten- ground in a modified Los Angeles abrasion test machine
sive gypsum and ettringite. Consequently, the hydration for 4  h of each 4  kg of ceramic powder. The grinding

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Table 1  Properties of OPC and ceramic powder aggregates and natural sand is illustrated in Fig. 1b and
Properties OPC Ceramic powder
compared with the limits specified by ASTM C33-13.

Chemical composition (%) 2.2 Mix Proportioning and Sample Preparation


SiO2 16.35 74.10
Al2O3 4.23 17.80 All mortar mixes were prepared with a binder-to-fine aggre-
Fe2O3 3.55 3.58 gates ratio of 1:2.75. The mixing was done at room tem-
CaO 68.28 1.13 perature of 25 ± 2 °C. The mix proportions of the mortar
K2O 0.23 2.65 were prepared based on the weight of materials following
TiO2 0.09 0.44 ASTM C1329-16. The water/cement (w/c) ratio used was
LOI 2.40 0.10 0.48 due to the appropriate workability and achieved the
Physical properties desired strength. In this study, two sets of mortar mixes were
Blaine fineness (cm/g2) 3990 4830 made so-called OPC and ceramic mixes. The OPC mix was
Specific gravity 3.15 2.53 designed as a control mix, whereas, in the ceramic mix, OPC
Soundness (mm) 1.0 2.0 was replaced by 40% ceramic powder and 100% fine ceramic
aggregates replaced the natural river sand. The proportions
of materials used in the mortar are revealed in Table 2.
process was continued until 90% of the powders passed Moreover, the flow table test was carried out on the fresh
through the sieve of size 45 µm following specifications mortar following ASTM C230-14. The OPC and ceramic
by ASTM C618-15. Based on the obtained chemical com- mortars were cast into cubical molds of size 50 mm for
positions of OPC and ceramic powder revealed in Table 1, assessing compressive strength test by ASTM C109-13. To
the ceramic powder used can be categorized as class F investigate the effect of chloride ions on the performance
pozzolans as the total ­S iO 2 + Al 2O 3 + Fe 2O 3 content is of mortars, the chloride penetration test was carried out.
higher than 70%. Also, Fig. 1a reveals the particle size The cubical specimens of size 100 mm were cast and then
distribution of waste ceramic powder and compared with immersed in 5% NaCl solution for up to 18 months. The
that of OPC. Moreover, the distribution of fine ceramic test procedure and the concentration of the solution were
followed by Higashiyama et al. [27]. After the designated

(a) (b)
100 100
OPC Fine Ceramic
Ceramic Powder ASTM C33-Upper Limit
80 ASTM C33-Lower Limit
80
Sand
Passing (%)

Passing (%)

60 60

40 40

20 20

0 0
0.01 1 100 10000 0.01 0.1 1 10
Particle size (µm) Particle size (mm)

Fig. 1  Particle size distribution of a OPC and ceramic powder; b sand and fine ceramic aggregates

Table 2  Mix design of OPC and Mortar mixes Cement Water Ceramic Natural sand Fine ceramic Flow test (mm)
ceramic mortars (kg/m3) powder aggregates

OPC 550 265 – 1460 – 145


Ceramic 330 265 220 – 1460 140

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Arabian Journal for Science and Engineering

immersion period, the mortar specimens were taken out and


then split into two parts. Soon after the splitting is done, the
inner surface of the specimens was sprayed by a silver nitrate
solution to observe the depth of penetration. Also, sulfate
attack test was carried out based on the ASTM C267-12. The
cubical mortar specimens similar to the chloride test were
immersed in 5% N ­ a2SO4 solution for the same immersion
period. The sulfate resistance was evaluated based on the
change in mass, dimensions and compressive strength of the
specimens after exposure.

3 Results and Discussion
Fig. 2  Compressive strength of OPC and ceramic mortars
3.1 Flow Test

The experimental findings of the slump flow test of both and it liberates calcium hydroxide (Ca(OH)2). This reac-
OPC and ceramic mortars are given in Table 2. The meas- tion is quite rapid. Nevertheless, when a pozzolanic material
ured flow diameter for OPC and ceramic mortars was such as ceramic powder is present, its reactive silica ­(SiO2)
145 mm and 140 mm, respectively. The ceramic mortar constituent reacts with liberated Ca(OH)2 in hcp (in the pres-
shows slightly lower workability as associated with the OPC ence of water) to form secondary C–S–H gels. This reaction
mortar. This was due to the angular shape of fine ceramic is relatively slow, causing a slow rate of heat liberation and
aggregates in addition to the finer particles of ceramic pow- slow strength improvement. This reveals that the pozzolanic
der than that of OPC particles. The addition of finer particles reaction consumes lime instead of producing it. Through the
such as ceramic powder into mortar and concrete mixtures development of extra C–S–H gels, the porosity reduced and
generally densifies the matrix by filling up the cavities and consequently resulted in higher strength of mortar at more
reduces the porosity. Consequently, it made the matrix stiffer extended curing periods [29].
and resulted in lower flowability of the ceramic mortar. The To attain a detailed understanding of the influence of
other studies on the utilization of waste ceramic aggregates ceramic powder on the hydration process, and strength
have also revealed that the workability of mortar and con- improvement of the mortar, the microstructural analysis in
crete mixtures reduced by the addition of waste ceramic terms of scanning electron micrograph (SEM) was applied.
particles [28]. The SEM images for OPC and ceramic mixes are revealed in
Fig. 3. It can be observed that in both OPC and ceramic mor-
3.2 Compressive Strength tars, the development of hydration products is significant.
Figure 3 further shows the C–S–H gels were more consist-
The measured values of compressive strength for OPC and ently formed and spared in the ceramic mortar as compared
ceramic mortars are demonstrated in Fig. 2. According to to that of the OPC mortar. Senthamarai et al. [12] and Rashid
the results indicated in Fig. 2, at the age of 7 days, the com- et al. [13] previously stated that the compressive strength of
pressive strength values of 41.8 MPa and 40.3 MPa were mortar and concrete increased with the replacement of OPC
recorded for OPC and ceramic mortars, respectively. Con- by ceramic powder as supplementary cementing materials.
cerning the results recorded, increasing in the curing periods
enhances the compressive strength values of ceramic mortar 3.3 Tensile Strength
specimens as compared to those of OPC mortar strength
values. For instance, at the ultimate age of 180 days, the The results of the splitting tensile strength for OPC and
ceramic mortar containing 40% ceramic powder and 100% ceramic mortars are shown in Fig.  4. A similar trend
fine ceramic aggregates obtained compressive strength of like that of compressive strength was detected in tensile
60.5 MPa which is about 8% higher than that of 56.2 MPa strength of mortar mixes containing ceramic powder and
recorded for the OPC mortar. fine particles. The splitting tensile strength of ceramic
The enhancement in the strength of the mortar compris- mortar was found to be increased with the increasing ages
ing ceramic particles might be attributed to the good poz- of curing. It can be attributed to the pozzolanic reaction
zolanic nature of ceramic powder, which contains a high arisen among the reactive ­SiO2 and Ca(OH)2, which was
amount of reactive ­SiO2. When OPC is mixed with water, it formed from the hydration process of the OPC. Besides,
forms a hydrated binding cement paste (hcp) of C–S–H gels, due to the pozzolanic nature of ceramic powder, the

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Arabian Journal for Science and Engineering

Fig. 3  SEM image of water-cured a OPC mortar and b ceramic mortar

5 3.4 Chloride Penetration
OPC Ceramic
4.5
4 The results of the chloride penetration test in terms of visual
Tensile strength (MPa)

observation, the mass change and microstructural analysis


3.5
of the OPC and ceramic mortar specimens exposed to 5%
3
NaCl solution for up to 18 months are describing in this sec-
2.5 tion. The surface color and texture of the mortar specimens
2 provide general information on the influence of chloride
1.5 on mortars; whether the color indicates the initial surface
1 or one causing from chloride attack. It has been observed
0.5
that in both OPC and ceramic mortar specimens, there are
no significant changes in the color and surface. The OPC
0
7 28 90 and ceramic mortars remain structurally intact without any
Time (days) visible crack or spalling on the surface of the specimens.
The results found in this study were comparable to those
Fig. 4  Splitting tensile strength of OPC and ceramic mortars reported by Senthamarai et al. [12], who pointed out the
positive influence of waste ceramic on the chloride resist-
ance of concrete.
splitting tensile strength values for the ceramic mortar at Figure 5 illustrates the variations in the mass of mortar
the age of 7 days were slightly lower than that of OPC specimens exposed to NaCl solution after 18 months. The
mortar [15, 30]. At the curing period of 7 days, the ten- outcomes show that both OPC and ceramic mortar speci-
sile strength value of ceramic mortar was recorded as mens revealed similar behavior, which raised the mass of the
2.85 MPa, which is about 4% lower than that of 2.95 MPa specimens by absorbing chloride particles. At the end of the
recorded for OPC mortar. However, at the longer curing immersion period, the mass of mortar specimens increased
periods, the splitting tensile strength of ceramic mortar by 3.8% and 2% for OPC and ceramic mortar mixes, respec-
increased as compared with the OPC mortar. For example, tively. It can be seen that the inclusion of waste ceramic
at the age of 90 days, the tensile strength of ceramic mor- as cement and fine aggregate replacement considerably
tar was found as 4.45 MPa, which is about 15% higher than prevented the mass gain of the mortars under the chloride
that of OPC mortar at the same curing time. The observa- attack. The drop in the mass gain of the ceramic mortar
tions made in this study were in agreement with the find- specimens might be attributed to the pozzolanic nature of
ings by Halicka et al. [15] and Medina et al. [16], which the ceramic powder. Due to the high amount of reactive
investigated the effects of fine ceramic aggregates on the ­SiO2 in ceramic powder, it can produce additional C–S–H
tensile strength of mortar. Their results show that with a crystals throughout the hydration process [2]. The additional
substitution percentage of 25% ceramic fine aggregates, C–S–H gels then make the microstructure of the specimens
the tensile strength increased by about 12% as compared denser and prevent the entry of disturbance particles such
to the reference concrete. as chloride ions and consequently improve the durability

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4.0 this reduction in the chloride penetration in the ceramic


OPC mortar mortar is due to the formation of the extra C–S–H crystals
3.5
Ceramic mortar which remains unchanged during the immersion period and
3.0 therefore improves the performance of mortar by providing
a dense microstructure [21].
Mass change (%)

2.5
Figure 7a, b shows the SEM image and EDX results of
2.0
OPC and ceramic mortars specimens exposed to chloride
1.5 solution after 18 months. The SEM images show the exist-
ence of more voids in the OPC mortar than that of ceramic
1.0
mortar specimen. Therefore, due to these pores in the OPC
0.5 mortar, the chloride ions penetrate faster into the specimens.
0.0 Also, the EDX analysis reveals the presence of chloride
0 5 10 15 20 mineral in the OPC mortar. However, there was no chloride
Immersion period (Months) mineral detected in the ceramic mortar owing to the denser
microstructure and lower porosity of the specimens. It can
Fig. 5  Mass change of OPC and ceramic mortars exposed to 0.5% be observed that the voids in the ceramic mortar are com-
NaCl solution paratively lower owing to the development of extra C–S–H
gels from the reaction among the S ­ iO2 of ceramic powder
and calcium hydroxide available from OPC cement hydra-
performance of mortar [31]. Also, the well distribution of tion. Moreover, the ceramic powder not only generates more
both ceramic powder and fine particles reduces the size of C–S–H gels but also act as fillers that reduce the amount and
the capillary pores and reduces the permeability of mortar size of pores in the matrix [32]. Ceramic fine aggregates
[3]. have also provided lower permeability in the mortar speci-
The depth of chloride penetration was determined by mens as compared to the natural river sand used in the OPC
using silver nitrate solution spray on the split face of the mortar [23, 33].
specimens immersed in the chloride solution. Figure 6 shows X-ray diffraction investigations demonstrated different
the split face of the mortar specimens exposed to NaCl solu- variations in the mineralogy of OPC and ceramic mortar
tion and then sprayed with the A ­ gNO3 solution to identify specimens exposed to chloride solution. Figure 8a, b reveals
the penetration depth. It can be observed that the portions the XRD patterns for OPC and ceramic mortar specimens
near to the surface of the mortar specimens were lighter in after 18-month immersion in chloride solution. It can be
color as a result of silver chloride, which is a white deposit observed that in the OPC mortar specimens before immersed
and indicated as the chloride penetration depth, whereas in chloride solution, the dominant peak was observed to be
the internal portions of the specimens were darker, owed the Ca(OH)2, which is the main hydration products of the
to the precipitation of silver hydroxide. The chloride pen- OPC cement. On the other hand, this peak was significantly
etration depth in the ceramic mortar was lesser than that reduced in the ceramic mortar, although the C–S–H gels
of OPC mortar. The average penetration depth of 15 mm peak was raised owed to the gradual pozzolanic reaction that
was recorded for OPC mortar, where only 5 mm depth of increases the resistance of mortar against aggressive envi-
penetration was recorded for ceramic mortar, which is about ronments. Generally, the severity peaks of Ca(OH)2 at 18 θ
67% lower than that of OPC mortar. As stated previously, and 47 θ scale in the XRD pattern decrease when cement is

Fig. 6  Split faces of a OPC


mortar and b ceramic mortar
specimens, which were treated
with ­AgNO3 after exposure to
chloride solution

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Fig. 7  SEM and EDX of a OPC (a)


mortar and b ceramic mortar
exposed to NaCl solution

Pores

(b)

Fig. 8  XRD patterns of a OPC mortar and b ceramic mortar exposed to NaCl solution

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Fig. 9  a OPC mortar and b


ceramic mortar specimens after
exposure to N
­ a2SO4 solution

replaced with ceramic powder. From the obtained results, it 4.0


can be seen that after immersion in the chloride solution, the 3.0
high peak severity of Ca(OH)2 content is vulnerable for chlo-
2.0
ride attack. In the OPC mortar specimens, the production

Mass change (%)


1.0
of gypsum was detected at 11 θ and 21 θ after immersion
0.0
in chloride solution. The results also show the formation of
-1.0
ettringite and thaumasite but in the lower amount than that
of gypsum resulting in less deterioration of the mortar. How- -2.0
OPC mortar
ever, there is no ettringite found in ceramic mortar sample -3.0
after 18 months of immersion, which was due to the lower -4.0 Ceramic mortar
porosity and water absorption of the ceramic mortar sample. -5.0
-6.0
Immersion Period (Months)
3.5 Sulfate Resistance
Fig. 10  Variation in the mass of mortar specimens exposed to the
Figure 9 displays the view of OPC and ceramic mortar speci-
­Na2SO4 solution
mens after 540 days of immersion in a 5% sodium sulfate
­(Na2SO4) solution. After the immersion period of 540 days,
the attack noted was a whitish precipitate on the surface ettringite, and thus reduces the specimen permeability and
of both the OPC and ceramic samples, but at a lower rate sulfate ion from penetrating the mortar specimen [20].
in ceramic specimens. This was due to the leaching and Figure 10 shows the test results of the mass loss of the
deposition of lime that was higher in quantity in OPC speci- mortar specimens under the sulfate attack. It can be observed
mens, and thus forming calcium sulfate (­ CaSO4). It can be that the entire specimens exhibited the same behavior
seen that there are no changes on the surface of the ceramic (change in mass) after immersion in N ­ a2SO4 solution. From
mortar specimens, while in OPC mortar specimen, a sig- the results, it can be seen that after 3 months of immersion
nificant surface deterioration was detected. The formation period, the mass of the OPC mortar was reduced by 0.7%,
of gypsum was observed in the OPC ceramic specimens while in the ceramic mortar increased by 1.7% as compared
due to the sulfate attack, which is the results of the chemi- to that of initial masses. The OPC and ceramic mortars
cal reaction among the sulfate solution and Ca(OH)2 in the show an increment in mass at the early ages of immersion.
Portland cement. However, in the ceramic mortar, there was However, the OPC mortar tends to reduce in the mass after
no significant change in the surface of the specimen. This 2 months of immersion by 5.1%. It can be due to the acceler-
might be owing to the pozzolanic nature of the ceramic pow- ation of sulfate attack, which leads to the formation of many
der, which provides a dense microstructure by the creation products from the reaction of sodium sulfate with cement
of extra C–S–H gels and results in high resistance against hydrates; thus, expand within the specimens. This expansion
sulfate attack [25]. Considerably higher ­C3A content in the is based on the formation of sulfate reaction products such as
OPC specimen should, in theory, make it more prone to sul- ettringite and gypsum that leads to cracking of specimens.
fate attack. Ceramic powders chemically bind the Ca(OH)2 Also, the mass gain in the ceramic mortar specimens could
in the form of calcium silicate hydrate (C–S–H), preventing be attributed to the sulfate reaction that increases the for-
Ca(OH)2 to react with sulfate and formation of gypsum and mation of gypsum and absorption of sulfate solution. The

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Residual compressive strength (%) 120 60


OPC mortar OPC mortar Ceramic mortar

Compressive strength (MPa)


Ceramic mortar 50
100
40
80
30
OPC: y = 49.219e-0.03x
60 20 R² = 0.9589
Ceramic: y = 54.396e-0.01x
40 10 R² = 0.9558
0
20 0 4 8 12 16 20
Immersion period (Months)
0
0 1 2 3 6 9 12 18
Immersion period (Months) Fig. 12  Compressive strength versus immersion period

Fig. 11  Residual compressive strength of OPC and ceramic mortars


exposed to N
­ a2SO4 solution period in ­Na2SO4 solution. From the results, it can be seen
that the strength of mortars reduces with the rise in the
immersion period. To demonstrate the effect of the immer-
reaction is known to cause an increase in the solid volume sion period on the strength of mortar, the power regression
of the system and may lead to the expansion of mortar [34]. method was used, with a coefficient of determination (R2)
A comparative strength value between the water-cured of 0.959 and 0.956, respectively, which signifies good confi-
specimens and specimen immersed in N ­ a2SO4 solution is dence for both OPC and ceramic mortars, respectively.
revealed in Fig. 11. The strength loss related to all mix- The formation of gypsum consequences in the deteriora-
tures was understood to be a consequence of the prolonged tion of mortar specimens by a drop in strength as well as
immersion into the N ­ a2SO4 solution. The difference in the expansion of specimens. The development of gypsum is
the strength between the companion specimen and those also recognized to be the initial step of ettringite formation
immersed in solution was considered as the strength loss. that considered as the major reason for mortar and concrete
It can be observed that the compressive strength of mortars deterioration under sulfate attack [25]. The SEM and EDX
is reduced with the increasing period of immersion. After images for both OPC and ceramic mortars are shown in
18 months of immersion period, the OPC and ceramic mor- Fig. 13a, b. It can be observed that the formation of ettrin-
tars show a reduction in compressive strength by 41.1 and gite was more significant in the OPC mortar specimens as
16.8%, respectively, as compared to the strength of speci- compared to that of ceramic mortar. The higher amount of
mens before immersion. The reduction in strength could be ettringite might be due to the higher amount of Ca(OH)2 pro-
attributed to the reaction between sulfate and Ca(OH)2 that duced during the OPC cement hydration process. The EDX
leads to the decomposition of cement hydration products and in OPC mortar sample displays the existence of gypsum and
therefore results in the reduction of strength. ettringite in the large quantity as revealed by the presence of
It was seen that mortar containing ceramic powder and Ca, O, Al and S. Nevertheless, different EDX spectrum can
fine aggregates obtained lower strength loss rate. This is be seen for the ceramic mortar specimen which consists of
attributed to the gradual pozzolanic reaction between the O, Si and Ca, where more C–S–H gels were produced by the
ceramic powder and Ca(OH)2, which caused in the devel- ­SiO2 of the ceramic powder and improved the performance
opment of additional C–S–H gels in the matrix. These of mortar under the sulfate attack.
additional hydrates, therefore, increase the density of the XRD analysis of OPC and ceramic mortar samples after
matrix and refine the pore structure. The utilization of fine 18 months of immersion in ­Na2SO4 solution demonstrated
ceramic powder to substitute cement not only reduces the different variations in their mineralogy, as illustrated in
amount of Ca(OH)2 in the matrix, but also the unreacted fine Fig. 14a, b. Similar outcomes like that of SEM and EDX
ceramic powder will act as a micro-filler and decreases the were obtained in the XRD patterns for both OPC and
gaps among the aggregates and binder, leading to a denser ceramic specimens. The results showed a high peak intensity
microstructure [35–37]. On the other hand, the utilization of Ca(OH)2 in OPC mortar sample before immersion, which
of ceramic powder and fine aggregates has empowered the leads to the production of the higher amount of gypsum and
manufacture of mortar with adequate resistance to sulfate therefore results in the formation of ettringite and thau-
and enhanced the performance of mortar by a reduction in masite in the OPC mortar. Thaumasite can also be formed
the strength loss. along with other calcium silicate hydrates during cement
Figure 12 displays the correlation among the compressive alteration, mainly when sulfate attack develops. Besides, the
strength values of OPC and ceramic mortars and immersion separation of peaks related to thaumasite and ettringite is

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Arabian Journal for Science and Engineering

Fig. 13  SEM and EDX of a


OPC mortar and b ceramic mor-
tar exposed to ­Na2SO4 solution

Fig. 14  XRD patterns of a OPC mortar and b ceramic mortar exposed to ­Na2SO4 solution

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Arabian Journal for Science and Engineering

greater at 2θ degree between 22 θ and 29 θ scale, as shown • The microstructural analyses of OPC and ceramic mor-
in Fig. 14a. The sulfate attack in mortar is generally recog- tars in terms of SEM and XRD revealed the variations
nized with the development of gypsum and ettringite crystals in the microstructure of both specimens exposed to the
[22]. Therefore, the increase in peak intensity of this mineral chloride and sulfate attacks. The voids in OPC mortar
shows the weak sulfate resistance and deformation of mortar. were increasingly filled up with other precipitated sub-
Due to the lesser volume of Ca(OH)2 in the ceramic mortar stance as a consequence of chloride and sulfate expo-
specimens, the produced amount of thaumasite and ettring- sure. Moreover, in the ceramic mortar, owing to the
ite was also comparatively lower than that of OPC mortar, pozzolanic behavior of ceramic powders and creation
but high peak intensity of C–S–H gel can be observed at of additional C–S–H crystals, mainly at longer curing
39 θ and 60 θ scale. This is due to the reaction of the silica periods, the pores fill up with the hydration products and
from ceramic powder with the excessive Ca(OH)2 from the consequently enhanced the microstructural, strength and
Portland cement hydration [35]. Figure 14b further reveals durability performance of mortar.
the high peak intensity of quartz in the ceramic mortar speci- • The possibility of replacing cement and fine natural aggre-
men even after 18 months of immersion, which indicates gate with waste ceramic particles produced by crushing
the existence of silica at high volume in the ceramic mortar waste from the tile industries offers technical, economic
specimens due to its good pozzolanic reaction. According to and environmental advantages which are of great impor-
Chen et al. [22] and Sotiriadis et al. [23], mortar containing tance in the present context of sustainability in the con-
ceramic particles had very high resistance to chloride and struction sector particularly as repairing materials.
sulfate attacks. Mohammadhosseini et al. [38] and Huseien
et al. [39] also demonstrated that the replacement of ceramic
powder and fine ceramic aggregates in mortar significantly Acknowledgements  The authors thankfully acknowledge the financial
support from Universiti Teknologi Malaysia (UTM) through Grant No.
increased the durability performance of mortar. Q.J130000.21A2.04E11.

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