Journal of Building Engineering 43 (2021) 102528

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Journal of Building Engineering

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Evaluation of the red mud and quartz sand on reinforced metazeolite-based

geopolymer composites
Yurdakul Aygörmez
Yildiz Technical University, Civil Engineering Department, Davutpasa Campus, Istanbul, Turkey

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

Keywords: In the production of geopolymer, which is an environmentally friendly material, it is important to use products
Geopolymer with different binding material potential. Zeolite, which is a natural and common, and low-cost material, and red
Metazeolite mud (RM), which is a by-product in the alumina refining industry, were used as binding materials. Calcined
Red mud
zeolite (metazaeolite (MZ)) was replaced with red mud in four different proportions (25%, 50%, 75%, and 100%
Quartz sand
High-temperature test
by wt.). Besides, standard sand was replaced with quartz sand (QS) as a different aggregate in five different
Freezing-thawing test proportions (20%, 40%, 60%, 80%, and 100% by wt.). The mechanical properties (compressive strength, flexural
strength, ultrasonic pulse velocity (UPV)) of the prepared 10 series were investigated in three different days (7,
28, and 56). In addition, the samples were subjected to the high-temperature test (250, 500, and 750 ◦ C) and the
freeze-thaw test of 400 cycles after 56 days. After the durability tests were completed, the strength, UPV, and
weight loss were determined. In addition, SEM analyzes were performed before and after the high-temperature
and freeze-thaw tests. According to the results, it was seen that the use of red mud at a rate of 25% contributed to
geopolymerization (a 12% increase in compressive strength) and showed this at the end of the durability tests. By
using quartz sand up to 40%, increasing the SiO2 ratio increased the results (a 30% increase in compressive
strength). Nevertheless, it was seen that stability for all samples was preserved after the durability tests.

1. Introduction cement significantly reduces CO2 emission [9].

The use of Portland Cement in concrete production is widely seen in
the construction industry. Because of the combustion of fossil fuels and
the calcination of limestone in the production of Portland Cement,
harmful gases and dust particles such as SO2, NO2, CO2 are released into
the atmosphere. In addition to such environmental problems, it requires
a significant amount of energy following aluminum and steel during the
production process [1]. Geopolymer is a binder produced by using
different industrial by-products in its production and constitutes an
important alternative to Portland Cement. Generally, sodium silicate
and hydroxide are used as alkali activators in geopolymer production,
and slag [2,3], fly ash [4,5] and metakaolin [6–8] are widely used as
binding materials. The waste material fly ash produced by thermal
power plants is used efficiently for geopolymer to reduce the carbon
footprint. Slag, which is densely found worldwide, is important waste
material and is obtained as a by-product in the metallurgical industry
and used in geopolymer production. Similarly, metakaolin produced by
calcining kaolin under high temperature is used extensively in geo­
polymer production. Substituting the geopolymer in concrete instead of
Red mud is an important by-product in the alumina refining industry
produced by obtaining alumina from bauxite ore [10–12]. During this
process, 240 ◦ C temperature and 1–6 atm pressure are applied and a
high concentration NaOH solution is used [12,13]. Approximately
1.5–1.6 tons of red mud is produced per ton of alumina production. It is
thought that red mud production is around 70 million tons annually and
the current state of global inventory is 2.7 billion tons [10–12]. The red
mud slurry is transported to waste lakes and subjected to water reten­
tion, and then drying and dewatering are applied to reduce maintenance
cost and volume [14]. These huge numbers occupy a significant amount
of land. The lack of systematic disposal of red mud against this condition
leads to an alarmingly serious environmental and economic problem. Si,
Al, and Fe oxides and hydroxides constitute the main composition in
general while processing conditions and bauxite origin affect the mud
composition. Besides its general composition, it has low proportions of
Na2O, TiO2, and CaO and it is alkaline by nature [14,15]. The particle
size of red mud is very thin, the presence of alkali and the high content of
iron limit the applications. Due to this situation, less than 5% are eval­
uated in specific industrial processes in several countries. Red

E-mail address: aygormez@yildiz.edu.tr.

https://doi.org/10.1016/j.jobe.2021.102528
Received 19 January 2021; Received in revised form 25 March 2021; Accepted 11 April 2021
Available online 19 April 2021
2352-7102/© 2021 Elsevier Ltd. All rights reserved.
Y. Aygörmez
mud-related research includes areas such as cement, glass ceramics,
brick making, crystal glazes, and metal extraction [15]. Despite the
studies on red mud, there is no widely accepted technology today.
Despite these situations, geopolymer technology as a potential field is
promising in this regard. Because it contains high levels of SiO2, Al2O3,
and caustic soda, which are very important in geopolymerization. In
addition, the fact that the geopolymer is important for the stabilization
of toxic substances and minimizing metals in red mud are the other
factors [16].
The use of natural zeolite as a precursor material for geopolymer
shows significant potential [17]. Sodium-based solutions (carbonate,
hydroxide, and silicate) were used for activation in the production of
geopolymer using raw zeolite. Due to their physical properties, the
highest results have been achieved with sodium hydroxide and hy­
droxide. The geopolymer concrete samples had a sufficient compressive
strength (16 MPa) and also had excellent adhesion properties. In the
case of curing at room temperature, slowly gaining strength was
observed, while the tendency to shrink was high [18]. While the high
water requirement of the zeolite was the factor in the high rate of
shrinkage, the high Si/Al ratio in the gel triggered the situation. Studies
on natural zeolite-based geopolymers have been investigated. Villa et al.
[19] suggested a curing temperature of 60–80 ◦ C in their study. Ulloa
et al. [20] produced pastes and mortars at 60 ◦ C curing temperature in
their study and obtained 17 MPa of compressive strength. Özen and
Alam [21] obtained 40 MPa of compressive strength by producing a
natural zeolite-based geopolymer sample. Unlike studies using sodium
hydroxide, Tekin [22] used zeolite, marble, and volcanic tuffs and ob­
tained compressive strength up to 46 MPa. In the case of curing in wet
conditions, efflorescence problems and cracks were observed. Also,
foaming materials such as H2O2 and Al powder and natural zeolite have
been used in the production of foamed geopolymer materials as insu­
lation material [23,24]. Metakaolin, produced by calcining kaolin be­
tween 600 and 900 ◦ C, is widely used in geopolymer production. It is
possible to apply the calcination method for natural zeolite. In this way,
it is seen that pozzolanic activity increases significantly. Claffy [25]
named the dehydroxylated zeolite as metazeolite. With the calcination
applied in this way, natural zeolites are made amorphous and more
susceptible to OH-attack. This has made it suitable for geo­
polymerization [26].
Quartz is the most important and most common mineral silica. Pure
quartz is colorless and transparent. While it mostly occurs in igneous
rocks, it occurs in almost all sedimentary and metaformic rocks. Its
formula is SiO2 and its basis is silica. Its hardness is 7 on the Mohs scale.
It is known to be quite durable according to mechanical and chemical
conditions. Due to this feature, while it is the dominant mineral in
mountaintops, it is also the primary component in river, beach, and
desert sand. Quartz is available in abundance everywhere and has the
property of durability. Sand is a scarce material in the world, so the
search for alternatives is important. Due to this feature, quartz sand,
which has higher strength than conventional concrete and creates some
additional advantages, is an alternative to fine aggregate [27]. Its
resistance to weather conditions paves the way for its use in buildings.
Quartz sand is used in the mining and railway industries for its traction
effect. Also, it is used in recreation in baseball, golf and volleyball courts,
beaches, and children’s sandboxes. It is also used in the oil industry and
glass production due to its corrosive effect. In addition, it is used as a
filler in the manufacture of paste, rubber, and paint. Having a higher
melting temperature than most metals allows it to be used as foundry
sand. In this way, it is also used as heat resistant. It is also used as re­
fractory brick, especially due to its high heat resistance [28,29]. Despite
these advantages, there are limited studies on the use of quartz sand in
geopolymer materials.
In this study, unlike other studies, red mud, an important by-product
obtained in the alumina refining industry, was also evaluated, while
using natural and common, and low-cost zeolite. Zeolite was primarily
calcined at 750 ◦ C and red mud was used as a substitute with the
2
Journal of Building Engineering 43 (2021) 102528
obtained metazeolite. While 100% metazeolite was used in the first se­
ries, red mud was used as substitutes (25%, 50%, 75%, and 100% by wt.)
in the other four series. Quartz sand was used as the aggregate in the
series with the highest results (25% red mud) in place of the standard
sand (20%, 40%, 60%, 80%, and 100% by wt.). The flexural-
compressive strengths and UPV results of 7, 28, and 56 days of the ob­
tained 10 series were found. In addition, 400 cycles (1 cycle consists of
12 h at + 20 ◦ C and 12 h at − 20 ◦ C) of freezing-thawing test and high-
temperature test consisting of 250, 500, and 750 ◦ C temperatures were
applied to see the behavior of the geopolymer samples against durability
conditions. After the durability tests, compressive and flexural strengths,
ultrasonic pulse velocity, and weight changes were found. In addition, a
visual inspection was made. Also, SEM analyzes were made before and
after the high temperature and freeze-thaw effects.
2. Materials and methods
2.1. Materials
The metazeolite used in geopolymer samples was produced by
calcining the zeolite at 750 ◦ C. The grain size of the metazeolite is 2–3
mm. The specific gravity of the metazeolite is 2.17 and its specific sur­
face area is 9660 cm2/g. The fine grain structure of the metazeolite and
the increase in the pozzolanic feature by calcining increased the degree
of geopolymerization. Red mud, as the name suggests, is the color of red
brick. The average particle size of the red mud is < 10 μm. Particles
larger than 20 μm are also available. The specific surface area of red mud
is 13.765 m2/g and its density is 1310.46 kg/m3. The chemical com­
positions of the two binder materials used are given in Table 1. Standard
sand in accordance with BS EN 196-1 was used for the first five series of
geopolymer samples. Quartz sand was used as a substitute for the other 5
series. The chemical composition of quartz sand is shown in Table 1.
Activators (sodium silicate (SiO2/Na2O = 3.29) and sodium hydroxide
(12 M)) were used for geopolymerization.
2.2. Geopolymer production and heat treatment
While preparing cementless geopolymer mortars, metazeolite, red
mud, standard sand, quartz sand, and sodium hydroxide and silicate
were mixed. While preparing the mortar, the aggregate/binder material
ratio was 2.5, the binder material/sodium silicate ratio was 1.5, and the
binder material/sodium hydroxide ratio was 3. For the mixture, firstly,
12 M of sodium hydroxide solution was prepared 24 h before and left to
cool. On the day of the mixing, sodium silicate and sodium hydroxide
solution were mixed. While preparing the activator solution, the sodium
hydroxide/sodium silicate ratio was taken as 1:2. The binder material
was then mixed with the activator solution using a mixer drill. After
mixing for 2 min, the aggregate was added, and mixing continued for 3
more minutes. The resulting mortar was put in molds and the vibration
was applied. It was then kept at room conditions at a relative humidity of
50% ± 4 and a temperature of 23 ± 2 ◦ C for 24 h. Then, the samples
taken out of the molds were placed in fireproof oven bags to prevent
water loss in the oven and kept in the oven at 60 ◦ C for 2 days. Samples
taken out of their bags after curing were kept in plastic storage boxes
until the test day. While 100% metazeolite was used in the first series,
25%, 50%, 75%, and 100% red mud were replaced in the next four se­
ries, respectively. Standard sand was used as aggregate for the first 5
series. In the next 5 series, quartz sand was replaced by 20%, 40%, 60%,
80%, and 100% for the binder with the highest result. Mixing ratios for
the prepared series are shown in Table 2.
2.3. Test procedure
Firstly, 7-day, 28-day, and 56-day compressive strength, UPV, and
flexural strength of the samples were found. Immediately after 56 days
were completed, the high-temperature and freeze-thaw tests were
Y. Aygörmez Journal of Building Engineering 43 (2021) 102528

Table 1
The chemical compositions of binding materials and quartz sand.
Chemical composition, % SiO2 Al2O3 Fe2O3 TiO2 CaO MgO K2O Na2O MnO L.O.I.

MZ 76.90 13.50 1.40 0.10 2.00 1.10 3.50 0.30 0.10 1.10
RM 14.77 25.18 34.90 5.24 1.81 0.26 0.30 9.13 0.07 8.34
QS 99.20 0.40 0.02 0.02 0.02 0.02 0.02 0.10 - 0.20

Table 2
Mixing proportions of geopolymer samples (%).
Mix ID Metazeolite Red Mud Standard Sand Quartz Sand

MZ 100 - 100 -
75MZ25RM 75 25 100 -
50MZ50RM 50 50 100 -
25MZ75RM 25 75 100 -
RM - 100 100 -
75MZ25RM20QS 75 25 80 20
75MZ25RM40QS 75 25 60 40
75MZ25RM60QS 75 25 40 60
75MZ25RM80QS 75 25 20 80
75MZ25RM100QS 75 25 - 100

applied to see the behavior of the samples against durability conditions.

The samples were kept for 1 day at 105 ◦ C for 24 h before starting the
high-temperature test. In the high-temperature oven, the temperature
increase rate per minute was set as 5 ◦ C. After the target temperature
was reached, the samples were held at a constant temperature for 1 h. Fig. 2. Flexural strength results.
Then the oven door was opened and the samples were cooled. The high-
temperature tests were applied with 250, 500, and 750 ◦ C. Also, 400
cycles of the freeze-thaw test were applied. 1 cycle consisted of 12 h at
− 20 ◦ C and 12 h at +20 ◦ C. At the end of durability tests, compressive
and flexural strengths, ultrasonic pulse velocity results, and weight loss
were found. Three samples were used for each test, and the data were
determined by taking the average of three samples. In addition, visual
inspections were made. Also, SEM analyzes were made before and after
the durability effects.

3. Results and discussion

3.1. Strength and UPV results

Results of 7-day, 28-day, and 56-day UPV, flexural strength, and

compressive strength of 10 series examined are given in Figs. 1–3. Clay
minerals are crystalline, raw material forms of clays and shales do not
show pozzolanic properties. However, they become calcined by heat
Fig. 3. UPV results.

treatment between 700 ◦ C and 900 ◦ C and acquire pozzolanic proper­

ties. Heat treatment disrupts the crystal structures of clays and shales
and turns them into a semi-amorphous shape or a degraded alumina
silicate structure. It has been observed that the geopolymer produced by
using metazeolite produced by calcining zeolite, a kind of clay mineral,
had significant strength and UPV results. The high content of reactive
alumina and silica in metazeolite increased the degree of geo­
polymerization and played a role in this situation. In this way, it has
become a binder material as a geopolymer precursor [26,30].
Strength values were changed with the addition of red mud. The
strength values increased with the addition of 25% red mud. In the case
of using 50% red mud, although the strength values were lower than the
sample without red mud, not much decrease was observed. The addition
of red mud created a peak behavior of 25% geopolymer strength.
Considering the results, it was seen that the contribution of red mud to
amorphous silica was very small. Despite this situation, the alkalinity of
the geopolymer mixture increased. While this situation accelerated the
dissolution of silica, it also increased the polymerization rate. Thus, it
Fig. 1. Compressive strength results.
has been observed that alkalinity constituted an important factor in the

3
Y. Aygörmez
geopolymerization process [31]. When a higher proportion of red mud
was used, the formation of shrinkage cracks increased. Cracks increasing
in number showed an enlargement when more than 50% red mud was
used. In addition, as the use of red mud increased, a more brittle fracture
formation was seen. The fine particle size and high specific surface area
of the red mud increased the ductility. Increased ductility in the case of
up to 25% use began to weaken at higher rates. These situations were
one of the reasons that caused the decrease in the mechanical properties
of the geopolymer. However, with increasing red mud, the amount of
inert material that was not effective in polymerization also increased.
This slowed down the polymerization process and caused weak matrix
formation [32,33]. Red mud allows toxic chemicals, heavy metals, and
radioactive waste to be encapsulated within the geopolymer network,
making them part of the polymer chain and hematite, which is highly
absorbent for heavy metals. Due to this situation, it acts as a cementi­
tious material and can be used in civil infrastructure applications such as
landfill areas and construction materials when used in geopolymer ap­
plications. The fact that it has a red color also allows it to act as a
warning in some engineering applications. It also helps to protect
environmental health by making use of waste materials [34]. Due to
these conditions, the peak value was seen at 25%, and its use of 50%
provided a significant advantage, although it decreased slightly
compared to the control sample.
When the effect of quartz sand in the series with the highest strength
in the first 5 series with 25% red mud was examined, the highest results
were found with 40% quartz sand. Having a high SiO2 content has made
a very important contribution to geopolymerization. It supported the
strengthening of the bonding degree by increasing the production of
Si–Al gel. Quartz sand has played an important role by reducing the
water absorption rate and pore structure and having a positive effect on
cohesion. Also, it strengthened the interface between aggregate and
matrix and acted as a buffer in front of cracks. When used at higher rates,
a decrease in strength has been observed in geopolymer gel binders since
they were not sufficient to maintain high compressive strength [35–37].
Compressive strength values at the end of 7, 28, and 56 days in
sample 75MZ25RM were 55.49 MPa, 58.87 MPa, and 56.96 MPa,
respectively. In sample 75MZ25RM40QS, the compressive strength
values were 65.49 MPa, 68.34 MPa, and 66.25 MPa, respectively. After
the 7, 28, and 56 days, the flexural strength values in sample
75MZ25RM were 9.68 MPa, 10.02 MPa, and 9.81 MPa, respectively. In
sample 75MZ25RM40QS, the flexural strength values were 10.77 MPa,
11.36 MPa, and 10.95 MPa, respectively. Within the scope of the study,
the change in the three-day strength results was also examined. While
there was an increase in strength results from 7 days to 28 days, there
was a decrease in the results in later days (56 days). The role played by
heat curing was important in this sense. The high-temperature effect
accelerated early strength gain. In this case, the high temperature
rapidly promoted the dissolution of solid binders and the formation of
reaction products and made a significant contribution. It has been
observed that the optimum temperature effect was effective in geo­
polymerization and strength development by managing the heat energy.
However, the rapidity of the reaction created negative effects on the
reaction products and microstructure in later ages. Puertas et al. [38]
stated that diffusion was an effective parameter in geopolymerization
and the reaction products would settle near to the particles of the binder.
With the advancing age, the microstructure homogeneity began to
deteriorate and a reduction in continuous reactions was observed. In
other words, while the dissolution of reactive products increased with
temperature, the microstructure became more dense and heterogeneous.
At first, the increased reaction products were replaced by delay over
time and diffusion became difficult. Due to this situation, the strength
increase was seen for up to 28 days and then decreased. However, the
geopolymer matrix had a compact structure and these reductions were
limited. The chemical structure of the gel significantly affected the
long-term behavior. The results are in line with the literature [8,39,40].
UPV tests were applied for investigating the continuity in matrices.
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Journal of Building Engineering 43 (2021) 102528
Increasing the number of voids in the material structure reduced the
speed of ultrasonic waves. However, there was a certain correlation
between unit weight and wave velocity. The penetration rate was
determined by considering the ratio of the distance between the source
point and the receiver to the elapsed time [41,42]. The increase in the
voids ratio increased the travel time and caused a decrease in the co­
efficient of ultrasonic sound penetration rate. The voids ratio signifi­
cantly affected the mechanical properties of concrete and mortars. In
this case, it was observed that red mud increased UPV values up to 25%,
and at higher rates decreased UPV values by decreasing workability [32,
33]. The inadequacy of quartz sand to provide high strength after 40%
caused a reduction in UPV values [35–37]. After the 7, 28, and 56 days,
UPV values in sample 75MZ25RM were 3468 m/s, 3524 m/s, and 3511
m/s, respectively. In sample 75MZ25RM40QS, the UPV values were
3589 m/s, 3637 m/s and 3615 m/s, respectively. According to the UPV
results, there was an increase in 28 days compared to 7 days and a
decrease after it. The reason that created this result was that its homo­
geneity was negatively affected and the gaps increased [8,39,40].
According to the results obtained, the correlation feature has been
investigated in order to investigate the compressive strength and UPV
compatibility and is given in Fig. 4. The R2 factor was found to inves­
tigate the degree of correlation. Since the R2 factor was 0.91 and higher
than 0.75, it has been observed that the compressive strength and UPV
results were consistent with each other. This indicated a satisfactory
correlation for all samples. The results of this study were also in line with
previous studies [6,8].
SEM analyzes were made to examine the microstructure formed in
the geopolymer composites. In this way, while the potential character­
ization created by the substitute materials was examined in detail, the
degree of the interfacial bond between the main and substitute materials
was also observed. SEM micrographs of samples MZ, 75MZ25RM, RM,
and 75MZ25RM40QS are given in Fig. 5. If the micrographs were
examined, parallelism was seen with the compressive strength results. It
was seen that the degree of homogeneity in the geopolymeric matrix
increased with the addition of 25% red mud. A good bond has been
formed between red mud and metazeolite. It was also observed that the
matrices in samples 75MZ25RM and 75MZ25RM40QS had continuity.
Air voids and micro-cracks were observed in sample RM. This indicated
that the compact structure was weakened by using 100% red mud. This
was caused by the deterioration of workability and homogeneity by
using 100% red mud [6,33–35].
3.2. Results of freezing-thawing effects
At the end of 56 days, the samples were subjected to a 400-cycle
Fig. 4. Correlation relationship between UPV and compressive strength.
Y. Aygörmez Journal of Building Engineering 43 (2021) 102528

Fig. 5. SEM micrographs of the samples: a) MZ, b) 75MZ25RM, c) 75MZ25RM40QS, and d) RM.

freeze-thaw test, and values of flexural strength, compressive strength,

UPV, and weight loss were found. Comparison of the results at the end of
the test and the 56-day results are shown in Figs. 6–9. A reduction in
strength values was found after the 400-cycles. Expansion of the water
present in the mortar due to freezing created a decrease in strength. At
the end of the frost formation, there was an increase of 9% in the water
volume in the mortar structure. This situation created hydraulic pressure
in the sample [43]. The formation of hydraulic pressure in the matrix
around the ice increased with the filling of empty areas. When the
effective force exceeded the tensile strength in the mortar structure,
micro-cracks and subsequent deterioration occurred. Due to this effect,
strength values also decreased [44,45]. Strength values before

Fig. 7. Residual flexural strength results after 400 cycles.

freeze-thaw testing affected the amount of micro-crack formation. Also,

the air voids ratio effect was important. Increased air gaps increased
UPV and strength loss [46].
But still, geopolymer samples showed significant resistance. This was
due to the compact structure and a good degree of adhesion that geo­
polymer matrices had. Also, the progress and development caused by the
effect of cycles in geopolymer matrices reduced losses. Freeze-thaw
working as curing at low cycles contributed to the formation of reac­
tion products and preservation of geopolymer integrity. While some of
the positive effects of the freeze-thaw test in the short term were strength
and dynamic modulus, it contributed to the activation of raw materials
Fig. 6. Residual compressive strength results after 400 cycles.

5
Y. Aygörmez
Fig. 8. Residual UPV results after 400 cycles.
Fig. 9. Weight loss results after 400 cycles.
(metazeolite and red mud) and increased resistance to hard frost con­
ditions. Since these effects occurring in short cycles did not fully reflect
the frost resistance of the geopolymer material, a long cycle of 400 cy­
cles has been evaluated [7]. The reason for the reduction in flexural
strength results was greater than compressive strength was that in
samples exposed to pressure load, cracks were in parallel with the
pressure load, while the damage consisted of flexural stress perpendic­
ular to the pressure load.
Using red mud at the rate of 25% increased the alkalinity and
increased the resistance and decreased the air gaps, increasing the
resistance to freezing attack [31]. Its use at higher rates decreased the
resistance against freezing-thawing by increasing the shrinkage cracks
[32,33]. Using 40% quartz sand contributed to geopolymerization due
to its high SiO2 content and this increased the resistance by increasing
the compactness. The use of quartz at a rate of 40% increased the
compactness of the sample as it reduced the visibility of the pores ac­
cording to the SEM analysis in Fig. 5. Also, quartz sand strengthened the
aggregate-paste interface, resulting in higher strength values [35]. After
the test in sample 75MZ25RM, the compressive strength, flexural
strength, and UPV values were 34.69 MPa, 4.65 MPa, and 2906 m/s,
respectively. In sample 75MZ25RM40QS, the compressive strength,
flexural strength, and UPV values after the test were 45.27 MPa, 5.81
MPa, and 3046 m/s, respectively.
After the freeze-thaw test was completed, it was determined that the
weight loss remained low. High and low cycle numbers affected weight
loss. Damp conditions in which the test was performed were effective in
low weight loss. Micro-crack formation at low cycles was effective in this
situation. After the formation of micro-cracks, the moist environment
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Journal of Building Engineering 43 (2021) 102528
contributed to the filling of gaps. Thus, weight increases were seen in
low cycles. While there was a movement towards the inside of the
sample due to the moist environment, there was also a movement to­
wards the outside of the sample. With the advancing cycles, deteriora­
tion and micro-crack formation increased. Along with the effect of the
number of cycles, calcification and peeling on the surfaces increased,
and weight loss also increased with this effect. This condition also
increased weight loss. However, the compact structure in the geo­
polymer still limited weight loss. The stable and homogeneous structure
was another reason that limited weight loss [7]. The structure, which
was more stable with the use of red mud by 25%, reduced weight loss.
Quartz sand also contributed to geopolymerization by using up to 40%,
which reduced weight loss. After the freeze-thaw test, weight loss was
found to be between 0.31% and 1.89%. The lowest weight loss occurred
in sample 75MZ25RM40QS, while the highest weight loss was in sample
RM. In this case, higher geopolymerization and lower voids ratio were
effective. The stronger aluminosilicate structure limited micro-cracks
and thus weight loss. Thus, weight losses were in parallel with
strength and UPV results.
After the freeze-thaw test, the sample surface was examined care­
fully. It was found that no serious damage was observed on the sample
surface after 400 cycles. The protected skin showed that the damage
remained at the level of micro-cracks. When the hydraulic pressure
resulting from the expansion of water by 9% exceeded the tensile stress
in the sample, micro-crack formation started and this situation remained
at a low rate. Visual inspection of samples after testing is given in
Fig. 10.
SEM micrographs of samples MZ, 75MZ25RM, RM, and
75MZ25RM40QS are given after the 400 cycles of the freeze-thaw test
(Fig. 11). Micro-crack formations were determined according to the SEM
images obtained from the geopolymer samples. The interface between
the gel and the metazeolite spheres facilitated the propagation of micro-
cracks and created a defective area. Despite these situations, the micro-
cracks were linked together for creating a network. The low rate damage
of the matrix was due to this situation. The slow progression of micro-
cracks also played a role in the limited decreases in strengths and UPV
results. The microstructure, which was weakened by the use of 100% red
mud before the test, was further damaged by the freeze-thaw effect.
Quartz sand, on the other hand, increased the durability by filling the
voids and creating a denser microstructure. As a result, the geopolymer
samples had high resistance against the 400 cycles effect. The results
were found to be consistent with other studies [47,48].
3.3. Results of high-temperature effects
The strength, UPV, and weight results at temperatures of 250, 500,
and 750 ◦ C were compared with the values at the end of 56 days and the
Fig. 10. Visual inspection after 400 cycles: 1) MZ, 2) 75MZ25RM, 3)
50MZ50RM, 4) 25MZ75RM, 5) RM, 6) 75MZ25RM20QS, 7) 75MZ25RM40QS,
8) 75MZ25RM60QS, 9) 75MZ25RM80QS, 10) 75MZ25RM100QS.
Y. Aygörmez Journal of Building Engineering 43 (2021) 102528

Fig. 11. SEM micrographs after 400 cycles: a) MZ, b) 75MZ25RM, c) 75MZ25RM40QS, and d) RM.

results obtained are given in graphs in Figs. 12–15. If the results were
examined in detail, a decrease in all mechanical properties including
strength values was observed. These decreases increased significantly
after 500 ◦ C. In this case, existing thermal reactions were effective. Due
to the reactions, dehydration occurred in the geopolymeric matrix along
with free water evaporation [47–49]. With advancing temperatures
(after 600 ◦ C) higher increases were seen in reduction rates. The steam
effect played an important role in the strength loss after 500 ◦ C. In fact,
the main reason for the loss of strength was the steam effect. With the
increase in temperature, the water present in the matrix structure turned
into steam. Above 100 ◦ C, the internal pressure increased continuously.
After the limit for steam pressure, the matrix began to condense with
little permeability. Due to this situation, the resistance decreased in the
face of thermal effects. Subsequently, thermal cracks formed on the
surfaces. Weight loss also increased because the evaporation of water
occurred in the matrix. Thermal shrinkage increased the cracks and at
the same time triggered weight and strength loss. High temperatures
also affected the aggregate-paste interface transition zone, creating Fig. 13. Residual flexural strengths after the high temperatures.
thermal incompatibility and causing micro-cracks [50]. In the alumi­
nosilicate gel structure, more crystallization was seen with the increase

Fig. 14. UPV results after high-temperature effects.

Fig. 12. Residual compressive strengths after the high temperatures.

7
Y. Aygörmez
Fig. 15. Weight-loss results after high-temperature effects.
of temperature. Thermochemical decomposition occurred in crystal
lattices due to crystallization stress. Renewal of the crystallization pro­
cess negatively affected the strength and ductility conditions. Due to the
deterioration of homogeneity, thermal incompatibility occurred and
micro-crack formation increased.
A strong geopolymer sample structure has gained importance in the
face of these effects. Having a strong character in the sample structure
allowed the heat to dissipate quickly and thus less thermal gradients
were formed. With this situation, thermal cracks and splits were limited.
Flexural strength results were more affected by high temperatures. With
the spread of cracks due to the increasing temperatures, the pore
structure grew and microstructural defects occurred. Microstructural
defects also significantly affected flexural strength [51]. Also, the
negative change in pore properties and workability affected the losses.
When the results after high temperature were analyzed in general,
similar behaviors as before the test were detected. The addition of 25%
red mud increased the alkalinity and contributed to the continuation of
geopolymerization and increased strength by reducing air gaps [31].
However, at higher rates, it reduced the resistance by causing shrinkage
cracks [32,33]. Quartz sand contributed to geopolymerization and
compactness by increasing the SiO2 content together by 40%. Also, it
provided higher strength values by strengthening the aggregate-paste
interface [35]. The compressive strength values in sample 75MZ25RM
at the end of 250, 500 and 750 ◦ C temperatures were 45.19 MPa, 33.48
MPa, and 18.44 MPa, respectively. In sample 75MZ25RM, the flexural
strengths after the 250, 500, and 750 ◦ C were 4.58 MPa, 2.57 MPa, and
1.51 MPa, respectively. The compressive strength values of sample
75MZ25RM40QS at the end of 250, 500 and 750 ◦ C temperatures were
57.14 MPa, 42.95 MPa, and 25.28 MPa, respectively. In sample
75MZ25RM40QS, the flexural strength after the 250, 500, and 750 ◦ C
were 5.54 MPa, 3.59 MPa, and 2.28 MPa, respectively.
If the UPV values were examined after the test, a decrease similar to
the strength values has been observed. These decreases reached higher
values with the temperature of 300 ◦ C. The deterioration in the solid
matrix triggered this situation. An increase in temperature increased the
water evaporation and also increased the growth of the pore structure.
This situation created additional gaps with weight loss. The increase in
gaps caused a reduction in UPV values by increasing the time required
for ultrasonic velocity waves to go between the source and the receiver.
At the same time, micro-cracks caused by temperature also caused a
reduction in the structure density and decreased the UPV values [52].
After the 250, 500 and 750 ◦ C in sample 75MZ25RM, UPV values were
2155 m/s, 1380 m/s and 956 m/s, respectively. In sample
75MZ25RM40QS, the UPV values were 2261 m/s, 1473 m/s and 1047
m/s, respectively at the end of 250, 500 and 750 ◦ C temperatures.
There has also been a significant increase in weight loss after high
temperatures. Water evaporation and dehydration caused by the heat
8
Journal of Building Engineering 43 (2021) 102528
formed in the geopolymer matrix caused microstructure damage and
subsequently, weight loss occurred. Weight loss consisted of three
separate stages. There was a loss of water that was physically absorbed
between 30 and 210 ◦ C. If it was between 210 and 400 ◦ C, there was a
breakdown in polymer side chains. In the main polymer chains, in­
terruptions occurred between 400 and 500 ◦ C. Weight loss increased
with these stages. It was higher at higher temperatures. Disturbances at
the aggregate-matrix interface also increased losses [53–55]. The use of
red mud up to 25% and quartz sand up to 40% increased compactness
and reduced weight loss. While the weight loss after 250 ◦ C temperature
was between 0.88% and 2.73%, it was between 2.96% and 4.65% after
500 ◦ C temperature. After 750 ◦ C, the weight loss was between 4.69%
and 7.11%.
Visual examination of the samples was made after 750 ◦ C tempera­
ture. Surface changes were examined and given in Fig. 16. The photos of
the samples were taken 1 h after the test was completed in the oven.
Color changes started to be seen on the surfaces in the photographs
taken at the end of 750 ◦ C. Damage to the geopolymeric main chains
increased the tendency of the sample surfaces to be slightly brittle and
rough. However, surface cracks remained limited. This situation showed
that the geopolymer samples preserved their stability after the high-
temperature effects [48].
SEM analysis was performed to see the changes in the structure of the
samples after 750 ◦ C high temperature. SEM micrographs of samples
MZ, 75MZ25RM, RM, and 75MZ25RM40QS after 750 ◦ C are given in
Fig. 17. Advances in micro-cracks were detected after high temperature.
When 100% red mud was used, air voids have started to form along with
the advancing micro-cracks. The main reasons for these situations were
matrix decomposition, weight loss, and phase transformations. The
resulting conditions increased the structural defects and the defect for­
mation was intensified on the continuation. Increasing defects also made
the structure more porous. In the case of using 25% red mud, the
strengthening of the bond grade increased the durability. The use of 40%
quartz sand strengthened the aggregate-matrix interface and supported
this situation. It was observed that the stable structure was generally
preserved despite these situations that occurred in parallel with the
decrease in compressive strength [47–49].
4. Conclusions
For this paper, metazeolite with red mud and standard sand with
quartz sand substituted were used, and the relevant results were found
according to the examination of the prepared geopolymer samples:
• According to the examination of the mechanical properties of the
prepared samples on three different days, it was seen that the heat
curing effect was positive between 7 and 28 days and then negative
(approximately 8% increase in compressive strength and then a 2%
decrease). With the application of high temperature as curing, there
was a positive effect on early strength, while a decrease in contin­
uous reactions and deterioration of the homogeneity of the micro­
structure occurred in later ages. Due to this situation, while the
results decreased after 28 days, these decreases were limited.
• The rate of 25% was a critical rate for replacing red mud with met­
azeolite. Peak behavior was observed with the use of 25% red mud.
In this case, the increase in alkalinity with red mud was a factor.
Thus, while the dissolution of silica was accelerated, the polymeri­
zation rate also increased (a 12% increase in compressive strength).
By using a higher rate, the amount of inert material that was not
effective in polymerization increased, while shrinkage crack and
brittleness increased and strength values decreased (compressive
strength reduction between 4% and 74%). Despite this situation,
when 50% red mud was used, it showed a very low decrease (a 4%
decrease in compressive strength) compared to the control sample.
• There has been an increase (a 30% increase in compressive strength)
of up to 40% in the substitution of standard sand with quartz sand. In
Y. Aygörmez Journal of Building Engineering 43 (2021) 102528

Fig. 16. Visual inspection with high-temperature effect (750 ◦ C): 1) MZ, 2) 75MZ25RM, 3) 50MZ50RM, 4) 25MZ75RM, 5) RM, 6) 75MZ25RM20QS, 7)
75MZ25RM40QS, 8) 75MZ25RM60QS, 9) 75MZ25RM80QS, 10) 75MZ25RM100QS.

Fig. 17. SEM micrographs of the samples after 750 ◦ C: a) MZ, b) 75MZ25RM, c) 75MZ25RM40QS, and d) RM.

this case, the increase in SiO2 content played an important role. The
increase in the production of Si–Al gel has strengthened the bond
degree with it. In this way, it also strengthened the aggregate-matrix
interface. At higher rates, insufficient gel-binder to sustain high
strength caused a reduction but still higher results were obtained
than the control sample (compressive strength increase between 14%
and 22%). According to the examination of the results, the lowest
result was in sample RM, while the highest results were in samples
75MZ25RM and 75MZ25RM40QS.
• After the high-temperature test and freeze-thaw tests, the strength,
weight, and UPV values of the samples decreased. While there was a
40% reduction in the freeze-thaw results, a 70% reduction was
observed in the high-temperature results. The test results were par­
allel to the pre-experiment situation. The progress of geo­
polymerization with the use of 25% red mud has kept the results
higher after the durability tests. Quartz sand has also increased the
resistance to durability tests by strengthening the aggregate and
matrix interface. Despite the decreases, geopolymer samples

9
Y. Aygörmez
preserved their stability at the end of both durability tests. Me­
chanical properties results are supported by analyzes results.
CRediT authorship contribution statement
Yurdakul Aygörmez: Conceptualization, Conception and design of
study, Funding acquisition, acquisition of data, Formal analysis, Data
curation, analysis and/or interpretation of data, Writing – original draft,
Drafting the manuscript, revising the manuscript critically for important
intellectual content, Approval of the version of the manuscript to be
published (the names of all authors must be listed).
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.
Acknowledgment
This work was supported by the research fund of the Yildiz Technical
University, the authors would like to express their sincere gratitude to
the scientific research coordination unit for their financial support to the
project (Project number: FAP-2021-4020).
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