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European Journal of Environmental and Civil Engineering
ISSN: (Print) (Online) Journal homepage: https://www.tandfonline.com/loi/tece20
Effects of alternative ecological fillers on the
mechanical, durability, and microstructure of fly
ash-based geopolymer mortar
Yosra Tammam, Mucteba Uysal & Orhan Canpolat
To cite this article: Yosra Tammam, Mucteba Uysal & Orhan Canpolat (2021): Effects of
alternative ecological fillers on the mechanical, durability, and microstructure of fly ash-
based geopolymer mortar, European Journal of Environmental and Civil Engineering, DOI:
10.1080/19648189.2021.1925157
To link to this article: https://doi.org/10.1080/19648189.2021.1925157
Published online: 13 May 2021.
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Effects of alternative ecological fillers on the mechanical,
durability, and microstructure of fly ash-based
geopolymer mortar
Yosra Tammam
a
, Mucteba Uysal
b
and Orhan Canpolat
b
a
Civil Engineering Department, Istanbul University- Cerrahpasa, Istanbul, Turkey;
b
Civil Engineering
Department, Yildiz Technical University, Istanbul, Turkey
ABSTRACT
In this research, the performance of fly ash/GGBS geopolymer mortars
made with different quarry waste powder as filler materials by substituted
the river sand fine aggregate with different ratios was evaluated based on
the mechanical, physical, durability properties and microstructural analysis.
Limestone waste, marble waste and basalt waste powder were used as
filler materials developing eco-friendly and economical geopolymer from
industrial waste as a promising sustainable area of research. A series of
tests were conducted such as on strength properties, ultrasonic pulse vel-
ocity (UPV), physical properties, abrasion resistance test, splitting tensile
strength and microstructure analysis (SEM). The samples were elevated at
the high-temperatures of 200 C, 400 C, 600 C and 800 C. Results con-
ducted that the use of limestone waste powder and marble waste powder
up to 50% ratio improved the geopolymer composite’s strength. The three
filler geopolymer composites positively affected water absorption, strength
properties and abrasion ratio results. The current article’s finding has indi-
cated a potential solution, presenting another geopolymer class followed
by the successful use of fly ash and quarry waste as significant asset mate-
rials. The output of this study is commercially expected to be effective
intercession for waste recycled and friendly environmental management
conclusions.
ARTICLE HISTORY
Received 12 November 2020
Accepted 28 April 2021
KEYWORDS
Fly ash; alkali activated
materials; lime waste
powder; basalt waste
powder; marble waste
powder; geopolymer;
high-temperature
1. Introduction
The extent of the cement factory’s greenhouse gas issue is caused by a visible growth in population,
infrastructure and industrial action, particularly in developing countries that produce a high request in
cement and concrete. The cement production in the cement factory has consumed much energy and cre-
ated vast amounts of carbon dioxide (CO
2
) emissions, which is greenhouse gas causing global warming
(Duxson et al., 2007; Imbabi et al., 2012; Meyer, 2009). However, the cement factory faces rising environ-
mental concerns with greenhouse gas emissions and the great energy-intensive despite the manufactur-
ing progress improvements. This industry is still responsible for a large proportion of the overall
greenhouse gas emissions into the atmosphere because mostly 7% of global carbon dioxide emissions
are being made by humans through cement factories (Billong et al., 2013; Dobiszewska et al., 2019;
Latawiec et al., 2018). Around the world, the binder in which geopolymers are a promising alternative is
being evolved as an eco-friendly candidate to decrease the latter’s use in concrete (Obonyo et al., 2014;
CONTACT Yosra Tammam yosra.tammam@ogr.iu.edu.tr Istanbul Universitesi, Civil Engineering, Fatih, 34452 Turkey
ß2021 Informa UK Limited, trading as Taylor & Francis Group
EUROPEAN JOURNAL OF ENVIRONMENTAL AND CIVIL ENGINEERING
https://doi.org/10.1080/19648189.2021.1925157
Olawale, 2013). Appealing geopolymer composites’properties are early development of strength, slight
pollution, and the percentage of high strengths to weight (Natali et al., 2011; Suraneni et al., 2014; Van
Jaarsveld et al., 1997). To begin the reaction of the polymeric bonds (Si-O-Al-O) active silica-alumina
source need. The alkaline solutions are the main components forming a geopolymer binder; then, the
resin is mixed with the filler material’s producing the binder (Lahoti et al., 2018). In the processing of
geopolymer sighting, SiO
2
and Al
2
O
3
as the principal oxides, industrial waste like fly ash, zinc slag, silica
fume, blast furnace slag, and red mud could be the suppliant of aluminosilicate that used in the geopoly-
mer matrix. Due to its commonality and availability worldwide, fly ash holds a significant role in the con-
struction section as pozzolanic by-product materials contribute to the production of binders with
excellent properties due to its commonality and availability worldwide. Therefore, its mechanical proper-
ties, durability assessment, and microstructural analysis were studied by many geopolymer researchers
(Abdulkareem et al., 2014; Aliabdo et al., 2016;
_
Ilkentapar et al., 2017; Khan et al., 2016; Koshy et al., 2019;
Nath et al., 2016; Nikoli
c et al., 2015; Singh et al., 2016; Wardhono et al., 2017; Zhou et al., 2020). Since
the fly ash (FA) based geopolymer is known for its lower carbon footprint, good mechanical characteris-
tics, durability, and high-temperature resistance properties, it emerged as an attractive alternative to
ordinary Portland cement (Davidovits, 1993,2008) What makes fly ashes, mainly class F fly ash, is the
right candidate for geopolymerization reactions: its contents, aluminate, and silicate. It is classified
depends on its composition, generally rich in SiO
2
,Al
2
O
3
, CaO and Fe
2
O
3
presented in the form of
amorphous and crystalline oxides or various minerals (Provis, 2014). Over the past decade, another envir-
onmentally friendly geopolymer inorganic binder has come into the spotlight, manufactured by alkaline
solution activating aluminosilicate source material. Its remarkable comparable performance with Portland
cement is the most promising Portland cement (Davidovits, 1989; Singh & Middendorf, 2020).
Since aggregates usually contain from 60 to 80% of the concrete’s volume, in attempts to change con-
crete into a more environmentally friendly production, designers may consider using aggregates in a
green way and replacing ordinary cement with green binders like geopolymer. Coarse or fine aggregates
are critical materials in concrete to improve the mechanical strength, volume stability, and inexpensive
materials; for centuries, river sand (RS) is being used as fine aggregate. It could be dredged from river
channels floodplains (Hunter et al., 2012). Qian & Song (2015) make a study using limestone powder as a
filler material focussing on the influence of limestone powder (0–30%) on the fresh and hardened proper-
ties of metakaolin based geopolymer, and they concluded their studies by stating that using of limestone
powder increases the strength properties and has an apparent positive effect on the flow of the mortars.
After the process of slicing marble fragments, an amount of waste is obtained. However, it is too high
for stocking, reaching millions of tons, and these wastes have unfortunately consistently been discarded
in open areas. There are three main problems caused by marble sludge: economic loss, environmental
pollution, environmental health, and thus, to provide an opportunity to obtain an environmental and
economic gain, we must reuse the waste of marble sludge, so it is suggested to use the marble waste in
concrete (Mashaly et al., 2016; Rana et al., 2015). Andr
e et al. (2014) and Martins et al. (2014) founds that
when marble waste is used in concrete as aggregate, the mechanical and durability properties could
improve. Turkey’s marble industry is considered one of the country’s largest industrial fields, counted by
millions of tons each year. Quarry industry leads to a vast amount of industrial waste out of the process,
and the search for ecologically reusing this waste is a priority. Other authors, such (Topc¸u et al., 2009),
(Bacarji et al., 2013) and (Corinaldesi et al., 2010), studied the influence of marble powder in concrete,
concluding that, up to given ratios of addition or replacement, concrete’s durability, and mechanical cap-
acity can be improved. Sreenivasulu et al. (2016) research the influence of using different ratios of filler
materials of fly ash-based geopolymer concrete on the mechanical properties. The study found that
increase the aggregate ratio to a specific limit could enhance and increase the strength properties, and
after that, mechanical properties start to decrease with the increase of aggregate ratio to binder ratio.
Also, the nature and properties of the aggregates such as hardness, thermal expansion coefficient, mech-
anical properties, and phase changes during heating are essential and critical parameters in composites
(Bernal et al., 2012). Earlier research proves that geopolymers concrete showed better results than
Ordinary Portland Cement specimen when exposed to elevated temperature, strength, resistance to
impact effects, and chemical attacks (Nath & Sarker, 2014; Rickard & van Riessen, 2014; Ryu et al., 2013;
Zhang et al., 2016). Other studies indicate that a geopolymer showed higher compressive and flexural
strength than (OPC) concrete (Sarker et al., 2014) and splitting strength after being exposed to excessive
temperatures (Junaid et al., 2015). Other studies tested geopolymer pastes and used F-class fly ash as
2 Y. TAMMAM ET AL.
binder material. To see how much loss of strength would be affected by thermal deterioration, they
exposed the samples to 800 C. The geopolymer mortar specimens had 65% less strength, whereas the
geopolymer paste specimens had 53% more strength. After reaching a temperature of 800 C, the aggre-
gate expanded by 1.5–2.5%, which led to a loss in strength (Kong & Sanjayan, 2008). Kong et al. (2007)
found that in fly ash geopolymer specimens, the density had increased, and a larger number of pores
had developed, which allowed water to evaporate. Moreover, after exposure to a high-temperature, the
geopolymer concrete has adequate strength and thermal-physical properties because of its ceramic-like
microstructures. Sakkas et al. (2015) apply successive severe thermal loading to geopolymer specimens to
study their performance under high-temperatures. They found that after applied high-temperature
(>800 C) to the geopolymer sample, they retained structural integrity, making this aluminosilicate mater-
ial a thermal barrier. To study the fire resistance, (Zhang et al., 2014) manufactured a geopolymer matrix
from fly ash F-class and metakaolin. The strength result was monitored under high-temperature condi-
tions, gave a new product that had better thermogravimetric and high-temperature resistance properties.
While the use of low calcium fly ash has been extensively investigated as raw material for the synthe-
sis of geopolymers in recent years, the study of using different waste fine filler material producing FA-
based geopolymer is limited. The core of this research to utilise the unused waste quarry dust like (LS,
MS, BS) offers green and high performance geopolymer. To investigate the effect of using the fillers with
different ratios flowing parameters were tested: flexural and compressive strength, splitting tensile
strength, abrasion resistance, ultrasonic pulse velocity (UPV) and microstructural analysis. Also, the mor-
tars’strength and microstructure properties under high-temperatures, ranging from 200 C to 800 C,
were evaluated. This research aimed to understand the performance of FA mortars using different quarry
waste aggregate and to provide a comprehensive and practical database for guideline modification,
engineering purposes, and further investigations on the field of FA geopolymers and alkali-acti-
vated mortars.
2. Materials properties
In this experimental study, geopolymer mortar was manufactured by using FA (Class F fly ash) related to
ASTM C618 (2010) standards. FA was supplied from Zonguldak/Turkey, while GGBS was supplied from
the cement factory in Bolu/Turkey. The chemical and physical composition for FA and GGBS were showed
in Table 1. The alkali activators to initiate the geopolymeric reaction process were sodium silicate and
sodium hydroxide (12 M). Both chemicals were obtained from AS Chemicals Company in Turkey. Their
technical can be seen in Table 2 and Table 3. In the control series, river sand (RS) were used as fine
aggregate with less than 0.25 mm particle diameter corresponding to TS 706 EN 12620 þA1 (2009). In
the three categories, the limestone powder (LS), waste marble powder (MR), and waste basalt powder
(BS) were used by partially replacing river sand in different ratios as affine aggregate. LS provided from
Gebze Rock Quarry/Turkey, BS was provided from INCI Group Company Sakarya/Turkey, and MR obtained
from Alibeykoy/Istanbul. The images of all filler materials used in this study are shown in Figure 1. The
chemical compositions and physical specifications of these fillers were illustrated in Table 4, as analyzed
Table 1. Chemical composition properties of (FA) and (GGBS).
Oxides SiO
2
Al
2
O
3
Fe
2
O
3
CaO MgO SO
3
Na
2
O free CaO Cl - LOI
Specific gravity
g/cm
3
Blaine
(cm
2
/g)
FA % by weight 54.08 26.08 6.681 2.002 2.676 0.735 0.79 0.11 0.092 1.36 1.98 2471
GGBS % by weight 40.55 12.83 1.10 35.58 5.87 0.18 0.79 —— 0.0143 0.03 2.90 2612
Table 2. Chemical properties of sodium hydroxide (%).
NaOH (g/kg) Na
2
CO
3
(g/kg) SO
4
Fe Cl Al
990 40,01 0.002 0.01 0.002
Table 3. Chemical properties of sodium silicate (%).
Na
2
O (%) SiO
2
(%) Density (20
o
C) (g/ml) Fe (%) Heavy metals as (pb) %
9.68 26.12 1.367 <0.005 35.8
EUROPEAN JOURNAL OF ENVIRONMENTAL AND CIVIL ENGINEERING 3
by XRF. As can be noticed from Table 4 main mineral of LS and MR is (CaO), while the main minerals of
BS are SiO
2
and AL
2
O
3
. The particle size distributions of filler material and river sand showed in Figure 2
and Table 5.
3. Experimental work
The series of geopolymer specimens were synthesised with FA (Class F fly ash) as a binder and adding a
fixed amount of about (13%) from (GGBS) mixed within the composites. Binder material FA activated in
alkali silicate solution. The sodium hydroxide solution prepared by adding 1 L of distilled water to 480 g
Figure 1. Filler materials a) Lime waste powder b) Marble waste powder c) Basalt waste powder.
Table 4. Chemical compositions and properties of filler materials.
Materials SiO
2
AL
2
O
3
Fe
2
O
3
TiO
2
CaO MgO K
2
ONa
2
O
Loss of
Ignition
Specific gravity
g/cm
3
Blaine
cm
2
/g
LS % 4.93 0.82 0.58 –51.97 0.58 ––40.40 2.79 2500
MR % 0.70 0.29 0.12 –55.49 0.23 1.80 2.44 42.83 2.71 8888
BS % 56.9 17.6 8.1 0.9 8.15 2.1 1.9 3.8 –2.76 6285
RS % 96.7 1.5 0.56 –0.08 –0.12 0.12 0.29 2.63 3500
Figure 2. The particle size distributions of filler materials.
Table 5. River sand gradation.
Grain size (mm) 0.16 0.5 1.0 1.6 2.0 2.0
Remaining (%) 99 88 71 35 5 0
4 Y. TAMMAM ET AL.
of sodium hydroxide pellets to obtain (12 M) prepared and stored at ambient temperature for at least
24 hours before being used. One-third of the activator mixture consisting of sodium hydroxide and two-
thirds of the activator mixture consisting of sodium silicate, the binder FA’s weight ratio to aggregate
materials was constant at 1:2. The activator to binder ratio for this mixture was taken at 0.75:1. Previous
trial experiments and earlier studies were used to prepare the mixture (Al-Mashhadani et al., 2018;
G€
orhan et al., 2016; Narimani Zamanabadi et al., 2019). Mixing compositions of produced geopolymer
mortars (kg/m
3
) were shown in Table 6. Fly ash was mixed with alkaline activator solution (mix of NaOH
and Na
2
SiO
3
), then slag added and mixed until the mixture became homogeneous. Next, the requested
amount of filler was mixed in fly ash paste, activated by the alkali solution as Figure 3 shown. The
obtained mixture was then cast into moulds to avoid the entrapped air and voids from the sample
moulds on the vibrator. After an hour of casting heat, curing was applied to all the specimens at 80 C
for 24 hours using an oven; the samples were kept in laboratory conditions until the scheduled tests.
Following the mixing procedure, 50 mm cube specimens were cast for compressive strength test and
physical tests, 40 mm x 40 mm x 160 mm prisms for flexural strength test and ultra-pulse velocity tests,
100 mm diameter and 200 mm height cylinders for splitting tensile strength, and cube specimens of
71 mm for Bohme abrasion test. Compressive strength test was obtained after 7, 28, and 56 days consecu-
tively the test applied according to ASTM C109/109M (2010). Flexural strength test was also obtained
after 7, 28 and 56 days consecutively test was done according to ASTM C348-20 (2020). An ultrasonic
pulse velocity test was carried on before the flexural testing on prismatic specimens to check the quality
of manufacture geopolymer specimens. The splitting tensile strength test of the geopolymer specimen
was determined by ASTM C 496 (2002). As specified in BS EN 1338 (2003) abrasion resistance test was
carried out on a cube specimen of 71 mm using Bohme abrasion test abrader, the loss in length (mm),
and weight (g) measurements were calculated due to abrasion. In this test, artificial corundum was used
as abrasive dust. After 28 days, the manufactured specimens have tested the effects of high-temperatures
of 200, 400, 600 and 800 C. samples were exposed to 105 C oven temperature for 24 hours before the
test applied to dry. The increment rate for temperature was 5 C/min; the samples were exposed to the
set temperature for one hour.
Table 6. Mixing compositions of produced geopolymer mortars (kg/m
3
).
Mix ID Fly ash GGBS Na
2
SiO
3
NaOH (12 M) River sand
Filler material
(LS or MR or BS)
Control 530 69 265 132 1060 0,00
25 LS 530 69 265 132 810,00 264,93
50 LS 530 69 265 132 560,27 529,87
75 LS 530 69 265 132 310,54 794,80
25 BS 530 69 265 132 807,30 264,93
50 BS 530 69 265 132 554,83 529,87
75 BS 530 69 265 132 302,38 794,80
25 MR 530 69 265 132 802,63 264,93
50 MR 530 69 265 132 545,52 529,87
75 MR 530 69 265 132 288,41 794,80
Figure 3. mixing process of the manufactured composites.
EUROPEAN JOURNAL OF ENVIRONMENTAL AND CIVIL ENGINEERING 5
4. Results and discussions
4.1. Strength properties
The effect of filler materials on the compressive and flexural strength of the manufactured geopolymer
specimen was determined, and the values are shown in Tables 7,8. In this study, the geopolymer
composite’s strength properties depend upon geopolymer gel’s strength and the interfacial bonding
between geopolymer gel and filler waste particles. Mainly the structure of the geopolymer mortar relay
on the Si/Al ratio formed by the leaching of Al
3
þand Si
4
. Previous study reported that using the Na
2
SiO
3
to the alkali solution could increase the Si/Al ratio which in turn could refine the pore structure of the fly
ash geopolymer (Ma et al., 2013). Findings show that using filler materials obtained a considerable
increase in flexural and compressive strength than the control specimen. The values obtained for com-
pressive and flexural strength yielded enhanced values in terms of time from 7 to 56 days, regardless of
the type of filler materials used. For instance, the categories of LS substituted with river sand in 25% and
50% ratio exhibited an achievement in flexural strength of percentage of 4.16% and 22.88% on the 56th
day, also in term of compressive strength increment of 5.57%, 8.72% compared to the control specimen.
The enhancement in strength properties for utilising LS is because utilising LS as calcium oxide rich
added substance dissolved and reacted in the solution for structure amorphous calcium silicate gel
hydrates (C-A-S-H), which existed together with N-A-S-H, the major geopolymer gel from polycondensa-
tion reaction. The finely ground LS added to the geopolymerization response since its partial dissolution
in an alkaline medium made it conceivable to expand the basic system of the geopolymeric binders. It
expanded the reactive stage, which expanded strength properties and diminished water absorption of
hardened mortar, including up to 50% LS. LS’s utilisation as a filler likewise makes it conceivable to fill
the pores inside the matrixes, clarifying LS’s significant impacts in the packing of particles in the geopoly-
mer matrix. Previous research on geopolymer (Bayiha et al., 2019; Embong et al., 2016) and cement con-
crete (D. Wang et al., 2018) also conclude that limestone powder’s addition improved the mechanical
properties. Additionally, for the MR category increasing marble waste powder ratio 25%, 50% content
Table 7. Compressive strength values at 7, 28, and 56 days (MPa).
Mix ID 7 Days GP 28 Days GP 56 Days GP
Control 61.90 –62.89 –65.12 –
25LS 63.65 2.83 64.25 2.16 68.75 5.57
50LS 66.91 8.09 68.09 8.27 70.80 8.72
75LS 58.41 5.63 60.67 3.53 63.91 1.87
25MR 63.30 2.27 64.10 1.92 66.76 2.52
50MR 64.66 4.47 65.99 4.93 67.80 4.12
75MR 53.56 13.47 56.65 9.92 57.10 12.32
25BS 62.80 1.46 64.67 2.83 67.55 3.73
50BS 52.67 14.90 53.20 15.41 55.60 14.62
75BS 50.20 18.89 51.20 18.59 52.80 18.92
Table 8. Flexural strength values at 7, 28, and 56 days (MPa).
Mix ID 7 Days GP 28 Days GP 56 Days GP
Control 10.33 –11.22 –12.26 –
25LS 10.73 3.87 11.88 5.88 12.77 4.16
50LS 13.94 34.96 14.58 29.90 15.07 22.88
75LS 9.82 4.94 11.96 6.55 12.87 4.98
25MR 10.80 4.55 11.49 2.41 12.57 2.53
50MR 10.90 5.57 11.22 0.00 12.65 3.18
75MR 10.70 3.63 11.22 0.00 12.08 1.47
25BS 10.60 2.66 11.33 0.98 12.65 3.18
50BS 8.70 15.74 9.20 18.00 9.26 24.47
75BS 8.66 16.13 8.99 19.88 9.20 25.00
Note GP (Growth Percentage) (%) ¼[(strength of specimen the strength of control specimen)/strength of control
specimen] 100%.
6 Y. TAMMAM ET AL.
showed an increment of compressive strength with 2.52%, 4.12%, the same as the flexural 2.39% and
1.93%, while 75% MR obtained decreases of 12.32% for compressive strength and slightly decreased
1.47% for flexural strength.
The increase in strength properties using MR is attributed to a significant silica amount, causing inter-
facial bonding between fly ash matrix and marble grains. At the same time, calcium (CaO) facilitates the
dissolution of aluminosilicates required for geopolymerization. The silicon dioxide present in FA responds
with calcium hydroxide present in MR framing calcium silicate hydrate network and conceivably contrib-
utes to the increment in the interfacial bonding in MR infiltrated geopolymer matrix. Comprehensively,
this improved interfacial adhesion yielded an increment in strength properties and diminished the geo-
polymer specimen’s water absorption. Marble waste powder has been used in many geopolymer research
(Colangelo et al., 2018; Thakur et al., 2019), and they found that it improves the mechanical properties of
geopolymers and reduces drying shrinkage. Also, concrete research (Alyamac et al., 2017; Binici &
Aksogan, 2018; Sardinha et al., 2016) used a waste of marble (sludge) and found enhancing the
strength properties.
On the other hand, the third categories of basalt stone powder with a ratio of 25% shows better
improvement than 50% and 75% ratios in compressive and flexural strength with a value of 0.56%,
3.18% respectively in comparison to control, in (Binici et al., 2020) previous study the addition of BS to
Figure 4. Compressive strength result of the manufactured composites.
Figure 5. Flexural strength result of the manufactured composites.
EUROPEAN JOURNAL OF ENVIRONMENTAL AND CIVIL ENGINEERING 7
the concrete was studied it showed that used BS in both powder and coarse aggregate effect positively
on the strength and abrasion of concrete. However, the BS is only filler, according to the (Laibao et al.,
2013). Therefore, it can be observed that the LS and MR were more efficient in promoting hydration in
the fly ash geopolymer matrix than BS (Figure 4 and 5).
4.2. Ultrasonic pulse velocity
A non-destructive test (UPV) is conducted to recognise the uniformity, quality of the geopolymer speci-
men, identify the probable defects, internal crack, and potential discontinuity of the manufactured
samples’material. Figure 6 shows the result of the UPV test. There is a slight growth between 7 and 28
values due to the similarities in the growth patterns; Figure 7 shows the UPV. Compressive strength cor-
relation with a coefficient (R2) 0.914 this value means that there is a strong correlation between UPV val-
ues are compressive strength results; this concludes that compressive strength behaviour could be
estimated by applying UPV tests. In this study, the filler materials affect the ultrasonic pulse velocity
measurement as previous articles found (Aarthi & Arunachalam, 2018; Musmar & Alhadi, 2008). Binici &
Aksogan (2018) mention that adding filler materials to the mixture decreases the water absorption and
porosity, so when the values of the void ratio decrease, the transition time for the ultrasound wave also
decreased, and the velocity will increase.
Figure 6. Ultrasonic pulse velocity values of the investigated mixes.
Figure 7. The correlation between UPV and compressive strength.
8 Y. TAMMAM ET AL.
4.3. Physical properties
Water absorption test obtained according to ASTM C140-07 on a 50 mm cube specimen, Table 9 shows
the produced specimen’s physical properties. Generally, the subsistence of replacement filler waste mate-
rials obtained a considerable improvement according to all of the transport properties inquired; this is
explained by the fineness particles of filler materials that help the geopolymeric matrix to had better
transport properties.
The (LS) categories result showed improvement in values compared to the control specimen by pre-
senting an increment percentage of 9.1%, 9.6%, 5.3% in terms of water absorption, as (Bayiha et al.,
2019) and (Wang et al., 2018) were found that adding LS improve the behaviour of absorbing water and
increase the density of the samples. The second categories that contain (MR) specimen obtain good
results compared to the control sample and (BS) categories. Samples of 25 MR, 50 MR mix display an
increment of 4%, 2.8%, in water absorption.
Whereas samples of 25BS, 50BS and 75BS showed 7.6%, 1.6 and 0.4% in terms of water absorption
respectively, previous studies on concrete made by. Sardinha et al. (2016) and Binici et al. (2020) mention
the same observation that using marble powder and basalt powder could improve the physical proper-
ties in concrete.
To check the consistency of fresh mortars before casting the workability of geopolymer paste were
measured. Flow table test were obtained by measuring the average diameter. The flow diameter of fresh
geopolymer was recorded in the range of 220–142 mm. Table 9 showed that control sample without
using filler materials indicates 224 mm flow diameter. Generally, the highest result was in the mixes using
ratio of 25% filler materials, while the lowest result was in the mixes using ratio of 75% filler materials.
4.4. Splitting tensile strength
Using waste materials as filler in manufacturing geopolymer influenced geopolymer’s tensile strength
(Amudhavalli et al., 2020; Zanvettor et al., 2019). Figure 8 illustrates the variation of splitting tensile
strength in 28 days and 56 days. The highest values splitting tensile strength in the 56 days were
6.14 MPa and 5.80 MPa related to 50 LS and 50 MR accordingly, while the control sample splitting tensile
strength was 5.41 MPa, so it is observed that LS and MR incorporated increases the splitting tensile
strength of mortars. A close observation of Figure 8 shows that 50% and 25% percent of LS, significantly
a percentage of 13.32% and 4.24%, considerably improve tensile strength than the control sample.
Besides, in the MR of ratio, 50% yielded the best results according to 25% and 75% compared to the con-
trol specimen, while the less obtained results about the replaced filler materials were the BS categories.
Furthermore, all the mixes are growing up in terms of time from 28 to 56 days.
4.5. Abrasion resistance test
The abrasion resistance is one of the critical problems of durability (Horszczaruk, 2005; Topc¸u & Canbaz,
2004;Y
€
uksel et al., 2006). Figures 9 and 10 illustrate the weight and length losses values correspondingly.
In general, all the analysed mixtures had a length loss of less than 2 mm and a weight change of less
than 3 g. The abrasion behaviour of the control sample is noticed to be the highest. The use of different
Table 9. The physical properties of the investigated mixtures.
Mix ID
Water absorption
(%)
Unit weight
(g/cm3)
Flow
(mm)
Control 8.64 2.23 224
25LS 7.85 2.32 191
50LS 7.81 2.33 157
75LS 8.18 2.32 145
25MR 8.29 2.26 186
50MR 8.39 2.26 153
75MR 8.7 2.20 140
25BS 7.98 2.30 215
50BS 8.5 2.32 201
75BS 8.6 2.31 194
EUROPEAN JOURNAL OF ENVIRONMENTAL AND CIVIL ENGINEERING 9
filler materials yielded an appositive effect either in length change or weight loss. However, it could be
connected to the subsistence of filler materials that own more abrasion resistance. Therefore, it produces
less length change and less weight loss. The filler effect of LS, MR and BS was mainly according to their
Figure 8. Splitting tensile strength values of the investigated mixes.
Figure 9. Abrasion losses per (g) values of the investigated mixes.
Figure 10. Abrasion losses per (mm) values of the investigated mixes.
10 Y. TAMMAM ET AL.
Figure 11. (a, b) SEM image for control specimen magnified 3000 and 5000 times; (c, d) SEM image for 50%limestone specimen
magnified 3000 and 5000 times; (e, f) SEM image for the 50% marble specimen magnified 3000 and 5000 times; (g, h) SEM image
for the 25% basalt samples magnified 3000 and 5000 times.
EUROPEAN JOURNAL OF ENVIRONMENTAL AND CIVIL ENGINEERING 11
particle size that they could fill the void in the geopolymer matrix and enhance the particle size distribu-
tion and finally increase the packing density of geopolymer composite that enhanced the compressive
strength and durability of geopolymer matrix. (LS) Categories indicate a convergent pattern according to
weight loss and length losses when it is checked against the control sample, same as (MR) categories, on
the other hand (BS) series yielded improvement less than LS and MR in length change, and weight loss.
Previous research found (Binici & Aksogan, 2018; Laibao et al., 2013) that using the MR and BS as filler
materials to the concrete decreases the abrasion resistance ratio, the same found in this study for fly ash-
based geopolymer.
4.6. Scanning electron microscopy (SEM)
Scanning electron microscopy was implemented for samples of higher given results: 50% LS, 50% MR,
25% BS, and the control sample as Figure 11 showed. Generally, all samples indicate a compact structure
and a homogeneous component with no cracks. Moreover, there is a particularly good degree of bond-
ing between the components of the matrix. From Figure 11(a, b), the micrographs for the control sample
observed there is some unreached (FA) appear; the uncreated Fa could improve the strength properties
according to earlier study founded (Ryu et al., 2013). Also, the gels (N-A-S-H) were formed. In Figure 11(c,
d), SEM image for 50% LS showed, previous researches (Valcuende et al., 2012; Wang et al., 2018 ) was
found that LS particle could fill the pores between hydration products and reduced the porosity in the
matrix. Also, the nucleation effect of LS could improve the hydration degree of binder and generate
more hydration products. From Figure 11(e, f), it observed Al and Si components that mean Al-O and Si-
O bonds are the primary chemical reaction that forms the matrix (Mehta & Siddique, 2017). In Figure
11(g, h) shows the SEM image for 25% BS, it is observed that the geopolymerization product gained and
the adhesion between BS particles and the matrix is also good.
4.7. High-temperature test
4.7.1. Weight loss after high-temperatures test
The ratio weight loss after elevated to high-temperatures for the manufactured specimens illustrated in
Figure 12. Generally, all the mixes showed weight loss less than the control specimen. It showed that
using the waste filler fine aggregates display a considerable improvement in the mixes where used.
Furthermore, the increased waste filler aggregate ratio was also found to enhance the geopolymer spec-
imens’weight loss performance when treated to high-temperatures. The increase in the temperature
made a dehydration reaction occurred in the geopolymer samples, made moisture inside the matrix
Figure 12. Weight loss ratio results after high-temperature exposure.
12 Y. TAMMAM ET AL.
reduces and moves towards the surface sample causing damage to the internal microstructure.
Consequently, degradation of the specimen is in terms of weight loss (Kong et al., 2007). The increase in
temperature increases the expansion of chunks’cracks, and expulsions cause the loss of strength and
weight ratio lead composite voids (Y€
uksel et al., 2011). The primary weight loss ratio that happens before
600 C from the geopolymer specimen has obtained value was from the evaporation of free water and
condensed hydroxyl groups (Wang et al., 2015). Furthermore, after heated up to above 600 C, the inter-
face reaction between fine filler aggregate and the geopolymer matrix caused the weight loss ratio.
These cumulative effects conclude that weight loss percentage increases in the specimens when tem-
perature increases in elevated high-temperatures test (Hiremath & Yaragal, 2018).
From Figure 12, weight loss ratios for the control specimen after exposure to high-temperature was
0.89% at 200 C, 3.15% at 400 C, 5.19% at 600 C, and 6.52% at 800 C. The weight loss ratios for LS geo-
polymer category were between 0.70% and 0.76% at 200 C, between 2.83% and 3.02% at 400 C,
between 4.16% and 5.30% at 600 C and between 5.55% and 6.13% at 800 C. Also, for MR category
Figure 13. Specimens after high-temperatures.
EUROPEAN JOURNAL OF ENVIRONMENTAL AND CIVIL ENGINEERING 13
weight loss ratios between 0.6% and 0.7% at 200 C, between 2.73% and 3.07% at 400 C, between
4.12% and 4.93% at 600 C and between 5.2% and 5.98% at 800 C.
The weight loss ratios for the BS category after exposure to high-temperatures were between 0.62%
and 0.75% at 200 C. And between 2.68% and 3.04% at 400 C, between 4.53% and 5.09% at 600 C, and
between 5.71% and 6.27% at 800 C. respect to the control specimen, LS, MR, and BS waste substitution
reduced the weight loss. These fine filler waste materials can decree the voids ratio to form a denser
structure (Uysal et al., 2018).
4.7.2. Visual inspection after exposure to high-temperature
Visual inspection of the specimens exposed up to 800 C was obtained immediately after the test was
done, as Figure 13 showed. Observing the specimens in which exposure to high-temperature saw a
change in their colour occurred (Celik et al., 2018). Figure 13 showed the specimen after exposure to
200 C, no considerable changes happen on their surface, and they did not have noticeable colour
change and protect their stable condition. However, the specimens after the high-temperature of 600 C,
the effect begins to be more apparent at 800 C, as Figure 13(d) showed the small cracks become appar-
ent and the specimens fragile, this is concerned to the destruction of the significant chains which form
the geopolymeric matrix composite.
4.7.3. Strength results
The resistance of elevated temperature for construction materials is one of the essential durability proper-
ties (Khaneghahi et al., 2018; Najafabadi et al., 2019; Zareei et al., 2019). Under the influence of high-tem-
perature 200 C, 400 C, 600 C and 800 C the specimens were examined and compared with 28 days
strength results, as Figures 14 and 15 illustrated. The losses in compressive and flexural strength results
after elevated to 600 C temperature started to show considerably decreases in strength properties, as
shown in (Tables 10,11). The major event that caused the reduction in strength properties related to the
thermal reaction after 600 C with the dehydration and water evaporated occurred (Zhang et al., 2012).
At elevated temperature, the aluminosilicate gel structure, be more crystallised. This condition leads to
the thermochemical decomposition of crystal lattices at the end of the crystallisation stress caused by
high-temperature. This inhomogeneous situation leads to thermal incompatibility. This is another reason
that caused the formation of micro-cracks. According to the observed result, the loss rate in flexural
strength was higher than the loss of the compressive strength result. This phenomenon occurred because
of imperfections, which brought about the spreading of cracks with the effects of high-temperature and
increase of pores (Zhang et al., 2016).
Figure 14. Compressive strength results after the high-temperature treatment.
14 Y. TAMMAM ET AL.
The reduction in compressive strength between 200 C and 800 C was with a range of 3.80–75.90%
for the control mix. With a range of 3.60–79.94% for LS series. With a range of 3.74–81.96% for the MR
series and within the range of 3.97–83.77% for BS series (Table 9). In terms of compressive strength, the
control mix performed 15.5 MPa at 800 C. The compressive strength results of 25 LS, 50LS, and 75LS
specimens at a temperature of 800 C were 17 MPa, 15.55 MPa, and 12.17 MPa. The compressive strength
results of 25MR, 50MR, 75MR specimen at a temperature of 800 C were 16.10 MPa, 13.77 MPa and
10.22 MPa, sequentially. The compressive strength values of 25BS, 50BS and 75BS specimens at a tem-
perature of 800 C were 14.87 MPa, 10.23 MPa and 8.39 MPa, sequentially. The obtained strength result
showed that 25LS, 25MR and 25BS performed better than the control mix when exposed to high-temper-
atures. At a higher replacement ratio of LS, MR, and BS, further higher strength losses after heat treat-
ment were observed as another research was founded (Uysal, 2012), the higher compressive losses were
observed in the BS series than MR and LS series.
Generally, similar results obtained by the test indicated a similar tendency to that of the specimens
before being exposed to high-temperatures as the LS mixes present better performance than BS and MR
mixes related to control series, the real damages of strength losses for geopolymer mortar happened
when the specimens exposed to an elevated temperature of 800 C. The good bonding of filler materials
with the geopolymer composite offers a good structural result under the effects of high-temperatures
along with high elastic modulus.
Flexural strength reduction rates at 200 C–800 C of manufactured geopolymer specimens were
between 4.10% and 76.11% for the control sample, within the range of 3.70–80.52% for LS series, within
the range of 3.83–83.96% for MR series, and within the range of 4.94–84.43% for BS series (Table 10).
Moreover, according to the manufactured geopolymer samples, the 25% replacement of filler materials
LS, MR, BS showed better performance reduction rates of flexural strength than 50 and 75 replacement
ratios. The flexural strength results of 25LS, 50LS, and 75LS specimens after high-temperature effect of
600 C were 6.89 MPa, 6.45 MPa, and 5.77 MPa, respectively. While 25MR, 50MR, and 75MR, the flexural
strength values were 6.05 MPa, 5.87 MPa, 5.0 MPa respectively at 600 C, and the flexural strength results
25BS, 50BS, 75BS were 5.87 MPa, 4.40 MPa, 3.75 MPa, respectively at 600 C. Furthermore, the differences
in thermal strain between paste and the fine aggregate caused the mortar matrix to deteriorate when
treated to high-temperatures between 600 C–800 C (Ameri et al., 2019).
4.7.4. Ultrasonic pulse velocity results
Figure 16 showed the UPV results after the high-temperature treatment. The water evaporation and
growth of pore structure in the geopolymer samples increase under the high-temperature effects. The
Figure 15. Flexural strength results after the high-temperature treatment.
EUROPEAN JOURNAL OF ENVIRONMENTAL AND CIVIL ENGINEERING 15
fall in the UPV test results was occurred by the mass loss causing the additional voids (
_
I. B. Topc¸u &
Karakurt, 2008). According to other samples, the limestone powder specimens proved better UPV results
under the high-temperature effects. Strength properties loss with an agreement to geopolymer matrix
indicated a significant decrease and dramatic damages and upon a large drop after 600 C elevated tem-
perature effects. The lower values obtained in the UPV test were after 800 C of high-temperature effects
due to the spreading time of UPV waves and the formation of some larger cracks. As Table 12 showed
the 25% of filler waste materials substitution as fine aggregates increased UPV results compared with
control samples, but when the substitution ratio increases up to 25%, the UPV result decreases. The con-
trol sample’s UPV value at a high-temperature of 800 C was 1453 m/s. The UPV results of 25LS, 50LS,
and 75LS specimens at elevated temperatures of 800 C were 2001 m/s, 2329 m/s, and 2155 m/s, sequen-
tially. The UPV values of 25MR, 50MR, and 75MR specimens at elevated temperatures of 800 C were
748 m/s, 1734 m/s, and 1892 m/s, sequentially. The UPV values of 25BS, 50BS and 75BS specimens at ele-
vated temperature of 800 C were 1803 m/s, 1633 m/s and 2204 m/s, sequentially.
4.7.5. SEM analysis
The SEM images for the heated specimens after 800 C were shown in Figure 17. It observed there was a
change in the material microstructure. The SEM image for unheated samples, as Figure 10, showed the
amorphous structure of the geopolymer composite with partially reacted FA particles encapsulated in the
matrix’s mass. This observation is compatible with other FA-based geopolymers found in the literature
(Temuujin et al., 2010).
A high porosity in the unheated specimens is visible. The porosity and high permeability in geopoly-
mer composite obtained a reduction of microcrack formation due to the path for the free water evapor-
ation (Temuujin et al., 2009). There were no more visible FA particles, and the bulk matrix appeared to
have transferred from an aggregation of particles to a continuous solid, this is consistent with the obser-
vations of another study (Yang et al., 2019). The formation of reaction products rich in silica gels makes
the pore volume dresses after high-temperature treatment, causing a high densification level to lead the
matrix structure to collapse as the increase in Si/Al ratio makes the initial densification temperature
decreases (De Silva & Sagoe-Crenstil, 2008).
Accelerated in pore volume mitigation, water losses, evaporation ratio, and dihydroxylation after
exposure to high-temperature could cause the structural failure or defects of formation intensifying.
These factors also contribute to the reduction of strength properties after high-temperature exposure.
Specimens that had good durability’s and thermal stability and refer to their zeolite-like structure (Zhang
et al., 2012).
The geopolymer matrix designs, filler type, aluminosilicate source type, alkali activator type, unreacted
alumina or silica, and other unreacted impurities determine the different types of characteristic peaks (Ye
Figure 16. UPV values after exposure to high-temperature.
16 Y. TAMMAM ET AL.
Figure 17. (a, b) SEM image for control specimen after exposed to 800 C elevated temperature magnified 500 and 3000 times;
(c, d) SEM image for 75LS specimen after exposed to 800 C elevated temperature magnified 500 and 3000 times; (e, f) SEM
image for 75MR specimen after exposed to 800 C elevated temperature magnified 500 and 3000 times; (g, h) SEM image
for75BS specimen after exposed to 800 C elevated temperature magnified 500 and 3000 times.
EUROPEAN JOURNAL OF ENVIRONMENTAL AND CIVIL ENGINEERING 17
et al., 2014). It can be concluded that there is a decree in strength in mortars that are subject to high-
temperature effects because of decomposition of gel, thermal incompatibility, and crystallisation.
5. Conclusions
In this research paper, the durability properties, mechanical properties, and microstructural analysis of
the manufactured samples of fly ash-based geopolymers mortars were investigated. River sand was sub-
stituted with different quarry waste filler materials. The study conclusions were as follows:
Results showed that the addition of LS and MR up to a 50% ratio enhanced the geopolymer
composite’s strength.
Due to abrasion, industrial waste filler’s existence improved the weight loss and showed better per-
formance as far as average abrasion is concerned. That is how the minimum abrasion ratio was
obtained for the LS category.
The use of industrial waste filler materials such as LS, MR, and BS in geopolymer mortars’production
improves the physical properties such as water absorption.
Table 10. Losses in the compressive strength after exposure to high-temperatures (%).
Mix ID 200 C 400 C 600 C 800 C
Control 3.80 14.53 45.13 75.90
25 LS 3.60 13.58 42.96 72.51
50LS 4.73 16.99 46.80 77.16
75LS 5.72 17.59 48.72 79.94
25MR 3.74 14.35 43.35 74.88
50MR 6.27 19.93 51.41 79.14
75MR 7.86 22.67 55.78 81.96
25BS 3.97 17.89 47.93 77.01
50BS 6.24 21.14 52.76 80.77
75BS 7.91 24.28 54.38 83.77
Table 11. Losses in the flexural strength after exposure to high-temperatures (%).
Mix ID 200 C 400 C 600 C 800 C
Control 4.10 18.00 47.59 76.11
25 LS 3.70 17.76 43.94 75.67
50LS 6.63 27.10 54.42 78.72
75LS 7.19 35.20 54.60 80.52
25MR 3.83 17.84 47.35 75.89
50MR 7.37 33.31 51.41 80.12
75MR 12.01 38.99 55.44 83.96
25BS 4.94 20.56 46.20 77.05
50BS 6.85 33.70 52.17 81.52
75BS 8.79 39.49 58.29 84.43
Table 12. Decreases in the UPV values after high-temperatures test (%).
Mix ID 200 C 400 C 600 C 800 C
Control 17.57 27.74 47.17 69.97
25 LS 16.96 27.10 46.26 68.24
50LS 17.49 27.54 46.54 68.33
75LS 18.16 28.53 48.12 70.60
25MR 16.62 26.88 46.25 68.47
50MR 17.37 27.49 47.75 69.66
75MR 19.55 29.98 49.68 72.27
25BS 18.02 28.23 47.52 69.65
50BS 19.64 31.86 51.07 73.63
75BS 19.89 30.58 50.78 73.95
18 Y. TAMMAM ET AL.
According to the SEM image, the geopolymerization mechanisms of the fly ash and alkaline solution
was good for all the categories and the control sample. Furthermore, the internal characteristics and
bonding between the geopolymeric matrix and the filler material were good.
The geopolymer matrix’s strengths properties considerably decreased in the temperature range of
600 C–800 C while the temperature increased. All the samples display similar behaviour and present
notable changes. There was a large droop in UPV values as the temperature went up to 600 C.
Cracks started to develop when there was a considerable loss in compressive strength at 600 C–
800 C range of temperature. There was a noticeable colour change in the geopolymer specimen
when the temperature exceeded 800 C. However, the cracks persisted at a lower rate, and this corre-
sponded to the fact that the geopolymer samples retained stable conditions under the effect of
high-temperatures.
The results of this research show a successful usage of industrial quarry waste material. This research
can create geopolymer composite materials by an eco-friendly process that is economically viable
and eco-friendly.
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
(Project number: FBA-2019-3558).
Disclosure statement
No potential conflict of interest was reported by the authors.
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