Ceramics International xxx (xxxx) xxx

Contents lists available at ScienceDirect

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

Shrinkage behavior and mechanical properties of alkali activated mortar

incorporating nanomaterials and polypropylene fiber
Mahmood Hunar Dheyaaldin a, *, Mohammad Ali Mosaberpanah a, Radhwan Alzeebaree b, c
a
Civil Engineering Department, Cyprus International University, Nicosia, North Cyprus, Turkey
b
Akre Technical Institute, Duhok Polytechnic University, Duhok, Iraq
c
Civil Engineering Department, Nawroz University, Duhok, Iraq

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

Keywords: Blended ground granulated blast slag (GGBS), low-calcium fly ash (FA), nano silica (NS), and nano alumina (NA)
Alkali activated mortar with/without polypropylene fiber (PPF) had a significant effect on the development length of alkali activated
Expansion mortar (AAM) cured at various humidity levels and curing ages. This paper presents the behavior of alkali
Drying shrinkage
activated mortar with 50% FA and 50% GGBFS binder materials and the alkali ratio of sodium silicate to sodium
Mechanical properties
SEM analysis
hydroxide (SS/SH) is 2.5. The molar concentration of sodium hydroxide (NaOH) used was 12 M. Feasibility
X-ray diffractions (XRD) Comparisons between the different humidity 60%–98% of at 23 ± 3 C◦ were examined. The strength behavior of
And durability alkali-activated mortar with different curing ages was also evaluated. Scanning electron microscopy (SEM)
analysis and X-ray diffractions (XRD) were also conducted to clarify the effect of nanomaterials and PPF on the
microstructures of AAM. It was found that the shrinkage values of AAM were decreased with the addition of
polypropylene fiber and nanomaterials. The combined use of both nanomaterials had better performance than
the use of nano SiO2 and/or nano Al2O3 alone. The combined use of PPF with nanomaterials had a superior
reduction in shrinkage and expansion and increment on strength values; the minimum shrinkage, expansion
values, and maximum strength were found at AAM mix incorporating 2%NS-1%NA-0.5%PPF. The SEM analysis
and XRD evaluation indicates the significant effect of nanomaterials on the microstructures and bond strength of
AAM. The microstructure of the mixes incorporating both nanomaterials and PPF was denser than other mixes
without nanomaterials and/or PPF and showed lower micro cracks.

1. Introductions development of alkali-activated materials in Western Europe in the

Shrinkage is a common cause of volume instability in concrete con­
structions. As a result of the shrinkage process, fractures occur. Concrete
can shrink due to moisture loss to the environment or interior drying.
The last causes early autogenous shrinkage, leading to significant in­
ternal stresses and fracture at an early age [1]. A variety factors influ­
ence the shrinkage behavior of alkali-activated concrete (AAC),
including aggregate quality, alkaline liquid and water concentration,
binder components, and curing environment. The alkali-activated con­
crete free of Portland cement was originally investigated in the 1940s
and drew a lot of interest from researchers. It was also widely used in
construction works in the 1960s [2] demonstrating that it might be used
by a greater number of individuals; Prof. Davidovits pioneered the
1970s [3]. The shrinkage strains are primarily influenced by the slag
cement composition and fineness, the type and amounts of alkali acti­
vator, and the curing conditions [1,4,5]. The shrinkage induced by
autogenous shrinkage was substantially larger in AAM specimens than
in OPC mortar specimens. The parameters of the alkaline activating
solution were found to be closely related to the degree of shrinking. The
magnitude of shrinkage is affected by solution properties such as Na2O
concentration and silica components [1]. The obtained data indicated
that the curing procedure used had an influence on all of the criteria
evaluated. After 28 days, the compressive strengths of the sealed-cured
specimens that had not been heat treated were greater when activated
with sodium carbonate. Heat-treated and unsealed specimens shrunk
more than sealed specimens, but a combined heat-treatment and

Abbreviations: AAM, alkali activated mortar; FA, Fly ash; GGBS, Ground granulated blast slag; NS, nano-silica; NA, nano-alumina; PPF, polypropylene fiber; OPC,
Ordinary Portland Cement; NaOH, sodium hydroxide; Na2SiO3, sodium silicate; XRD, X-ray diffractions; SEM, scanning electron microscopy.
* Corresponding author.
E-mail address: mahmood.dheyaaldin@gmail.com (M.H. Dheyaaldin).

https://doi.org/10.1016/j.ceramint.2022.04.297
Received 6 March 2022; Received in revised form 20 April 2022; Accepted 25 April 2022
Available online 29 April 2022
0272-8842/© 2022 Published by Elsevier Ltd.

Please cite this article as: Mahmood Hunar Dheyaaldin, Ceramics International, https://doi.org/10.1016/j.ceramint.2022.04.297
M.H. Dheyaaldin et al. Ceramics International xxx (xxxx) xxx

Table 1
Chemical composition and physical properties of fly ash (FA) and ground granulated blast slag (GGBS).
Component CaO SiO2 Al2O3 Fe2O3 MgO TiO2 SO3 K2 O P2O3 Mn2O3 Na2O SrO L.oI

FA% 15.48 48.43 17.15 11.96 1.35 2.68 0.82 0.41 0.4 0.17 0.0019 0.2 1.47
GGBS% 47.75 28.17 8.6 0.42 3.89 0.94 1.45 0.29 0.06 0.47 0.02 0.076 0.2

higher structural applications. According to studies, the amount of oxide

Table 2
in the binder materials and activator has a significant impact on how
Properties of nano materials and Polypropylene fiber (PPF).
effectively it performs at high temperatures. The range of AAC’s binder
Additives Particle size Purity Color Shape compositions makes it difficult to determine the mechanisms that cause
Nano silica (NS) 20–30 nm 99.8% White Amorphous change in characteristics, which is one of the obstacles in evaluating the
Nano alumina (NA) 20–30 nm 99.9% White Gamma behavior of AAC at high temperatures. Furthermore, because of the
Polypropylene fiber (PPF) 13 μ (Ø) and 6 mm – –
variety of study methods, comparing results with others is difficult [7].
Several studies studied the production of alkali-activated concrete and
mortar using by product of (FA) fly ash and (GGBS) ground granulated
Table 3 blast slag. The production of alkali-activated concretes significantly re­
Properties of natural fine aggregate. duces the industrial waste by at least 12.2 million tons per year while
Properties of Natural Sand emitting five to six times less CO2 [8,9].
Fine Modulus of fine aggregate 3.09
The yearly worldwide ash production is around 500 million tons,
Bulk density of aggregate (U = A/V) 1612 kg/m3 with fly ash (FA) accounting for 75–80% of it. Due to the disposal issues
Bulk specific gravity- dry basis 2.71 associated with fly ash (FA), researchers have started to utilize it in the
Voids Ratio; Vd = 100*(S*D-U)/(S*D) 40.2 production of Portland cement. As a result, some researchers have
Absorption % =(B-A)/A*100 0.6
focused their efforts on developing cement-free concrete, also known as
alkali activated concrete, utilizing fly ash (FA) as a raw material [10,11].
All of these issues have encouraged researchers throughout the world to
develop novel, simple-to-use, and ecologically friendly building mate­
rials that consume less energy and emit less carbon dioxide. These ma­
terials may be used with a variety of wastes while still performing as well
as characteristic of Portland cement structures [12].
Geo-polymerization, also known as alkaline activation, and it is a
chemical process that turns an amorphous structure into a completely
cementitious composite. The higher strength qualities are due to dense
of structure. The development of normal and high strength AAC cured at

Table 5
The variable ranges of additives.
The variables range

Variables Assigned Level of Variables

Fig. 1. Sieve analysis of natural fine aggregate.
− 1 0 1

Nano silica NSa 0.0% 1.0% 2.0%

sealed-curing process exhibits lower shrinkage values by 30–50% in all Nano alumina NAb 0.0% 1.0% 2.0%
conditions. The reduction was caused by beginning of a more extensive Polypropylene fiber PPFc 0.0% 0.5% 1.0%
hydration/geopolymerization process, which resulted in a denser binder a
Friction of binder material addition.
matrix with higher tensile strength [6]. Efforts have been conducted to b
Friction of binder material addition.
better recognize the properties of AAC and to develop mixtures with c
Friction of fiber addition.

Table 4
Mix design and quantity of material.
Mix No. Mixes NS NA PPF FA GGBS S.H S.S F. Agg SP E.W
kg/m3 kg/m3 kg/m3 kg/m3 kg/m3 kg/m3 kg/m3

M1 NA2 − 1 1 − 1 343 343 100 250 1033.5 21 33.35

M2 NA2-PP1 − 1 1 1 343 343 100 250 1033.5 21 33.35
M3 PP1 − 1 − 1 1 350 350 100 250 1033.5 21 33.35
M4 NA2-NA2 1 1 − 1 336 336 100 250 1033.5 21 33.35
M5 NS2-NA2-PP1 1 1 1 336 336 100 250 1033.5 21 33.35
M6 NS2 1 − 1 − 1 343 343 100 250 1033.5 21 33.35
M7 NS0-NA0-PP0 − 1 − 1 − 1 350 350 100 250 1033.5 21 33.35
M8 NS2-PP1 1 − 1 1 343 343 100 250 1033.5 21 33.35
M9 NS1-NA1 0 0 − 1 343 343 100 250 1033.5 21 33.35
M10 NS1-NA2-PP0.5 0 1 0 339.5 339.5 100 250 1033.5 21 33.35
M11 NS11-NA1-PP1 0 0 1 343 343 100 250 1033.5 21 33.35
M12 NS1-PP0.5 0 − 1 0 346.5 346.5 100 250 1033.5 21 33.35
M13 NA1-PP0.5 − 1 0 0 346.5 346.5 100 250 1033.5 21 33.35
M14 NS2-NA1-PP0.5 1 0 0 339.5 339.5 100 250 1033.5 21 33.35
M15 NS1-NA1-PP0.5 0 0 0 343 343 100 250 1033.5 21 33.35

2
M.H. Dheyaaldin et al.
Fig. 2. AAM specimen at different humidity.
high temperatures has been the emphasis of the production of AAC for
the past two decades [13]. In the recent decades, the focus of research
has switched to the production of AAC cured at ambient temperature in
order to reduce the amount of energy required for curing [14,15].
Researchers are becoming more interested in using nanoparticles in
AAC to increase mechanical properties. Many studies on the usage of
nanoparticles to improve the mechanical properties of AAC have been
conducted [16–19]. The addition of nano alumina to pozzolanic binders
produced a novel behavior. Except the volume change of the specimens,
alumina nanoparticles significantly enhanced almost properties of AAC.
The development of C-A-S-H molecules can adequately ex-plain this
phenomenon. Nanoparticles composed of alumina not only represent as
a filler to hold the microstructure together, but they also appear to have
a beneficial impact on the formation of these compounds [20]. The
contribution of NS to the lime–pozzolan and lime–metakaolin compos­
ites enhanced their compressive strength. Moreover, in both composites,
NS inhibited carbonation and water absorption while also providing
denser microstructures [20].
Polypropylene fibers (PPF) have been demonstrated to inhibit plastic
shrinkage cracking; However, as far as the authors are aware, they have
not been studied control the drying shrinkage cracking utilizing the
linear type of restricted shrinkage test [21]. The evaporation of free
water in concrete causes drying shrinkage, which is directly related to
the characteristics of the binder paste, where the porous matrix, espe­
cially the form and size of the cavities, are the most essential concerns.
Consequently, rewetting concrete will not improve drying shrinkage
[22,23]. Micro polypropylene fiber (MPPF) was used at five different
volumetric percentages: 0%, 0.50%, 1%, 1.50%, and 2%. It was noted
that the MPPF content was selected based on previous studies [24].
When compared to steel fibers, polypropylene fibers (PPF) are the most
commonly used commercial fibers due to their low cost and corrosion
resistance [25]. PPF also has a significant advantage over other synthetic
fibers, including their low thermal conductivity, lightweight character­
istics, and resilience to acid and alkali attacks [26].
Alkali activated concrete is produced with an alkali-activated solu­
tion and alumina-silicate-based components. The cost and availability of
alkali-activated solutions and alumina-silicate-based materials both
have a factor in their selection. Slag and fly ash are two examples of
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aluminosilicate sources [27–30]. However, researchers recently focused
on the utilization of nanomaterials and fibers to improve the properties
of AAC [31–35]. It was illustrated that the addition of 2% nano-silica by
weight of binder materials was the optimal percentage for complete the
geopolimerization process and acting as a cavity filler; however, it was
significantly dependent on the base materials used [31,33]. The me­
chanical properties of AAC were not increased by increasing the con­
centration of nano-silica more than 2% by weight. This was due to the
fact that the inclusion of nano-silica resulted in poor dispersion between
the nano-silica and the matrix, resulting in micro void formation, which
weakens the AAC matrix [36].
On polypropylene fiber (PPF) reinforced concrete, the impacts of
nano-alumina (NA) and rice husk ash (RHA) were investigated [37].
Nano-alumina (NA), polypropylene fiber (PPF), and rice husk ash (RHA)
were added to mortars to reduce water absorption and drying shrinkage
while simultaneously improving flexural strength [38] Slag concretes
containing 0.2% and 0.5% volume fractions of PPF fibers had lower
cracking resistance than those without fibers due to the combined effect
of higher elastic modulus and higher drying shrinkage. Drying shrinkage
was influenced by the fiber’s elastic modulus, as well as its size and
volume percentage [38]. The drying shrinkage values of all prepacked
aggregates fiber-reinforced concrete (PAFRC) specimens reinforced with
waste polypropylene fibers were lower than those of plain prepared
aggregate concrete (PAC) [39]. The highest reduction in the drying
shrinkage of the PAFRC pumping mix method with 0.75% fibers was
found to be 29.5% smaller than that of the plain mix [39]. The results are
interpreted as a growing rate until the age of 21 days, followed by a
stable rate of change. For fiber reinforced composites, the 84th-day
drying shrinkage values ranged from 187 to 335 micro strains [40].
It’s worth mentioning that all the specimens had a drying shrinkage of
less than 500 micro strains standards at the age of 28 days. According to
the findings, polypropylene and polyvinyl alcohol fibers had a signifi­
cant impact on drying shrinkage. PPF has the ability to reduce concrete
creep and shrinkage [41]. Drying shrinkage is most common during the
early phases of development. AAS pastes have a larger drying shrinkage
than AAS mortars. Meanwhile, it was noted that AAS mortars exhibited
more drying shrinkage than comparable Portland cement mortars [42].
The flexural tensile strength of fiber-reinforced geopolymer mortar
M.H. Dheyaaldin et al.
Fig. 3. Molds of length change test with detail dimensions.
(FRGM) for 3 days, 7 days, and 28 days with different PP fiber contents.
The flexural strength of the specimens at 3 days increases as the fiber
concentration increases and polypropylene PP-1 achieves a maximum of
3.6 MPa, which is 12.5% higher than the control specimens [43]. The
highest flexural strength after 7 days is 4.1 MPa, which is greater than
the control specimens by 20.6%. The compressive and flexural strengths
of a 3% nano-SiO2 and nano-Al2O3 mixture were 48.1 and 46.1 MPa,
respectively, while the compressive and flexural strengths were 5.23 and
5.26 MPa, respectively [35]. When nano-alumina is added to an AAC
mix, the geopolymerization process improves, and mechanical perfor­
mance improves, then decreases as the alumina concentration increases
due to the weakening bond effect [44]. Polypropylene (PP) fibers are
added to the mortar at ratios of 0.5 and 1% by volume. The addition of
0.5% and 1% polypropylene PPF to slag-based fiber-reinforced alkali
activated mortar (FRAAM) had no effect on compressive strength at age
of 2 and 28 days. However, the compressive strength of fly ash-based
FRGAAM at age of 2 days was enhanced due to higher PPF content. At
age of 28 days, the same composite shows an opposite tendency. A
significant improvement in compressive strength at both ages was noted
due to incorporation of PPF to slag/FA based FRAAM [45].
Although there are studies about the combined use of nanomaterials
and PPF for conventional concrete. There are rare or a few studies
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Ceramics International xxx (xxxx) xxx
regarding the shrinkage behavior and mechanical performance of AAC.
The goal of this study is to find out the shrinkage behavior and me­
chanical characteristic of alkali activated mortar incorporating nano
materials (nano-silica, and nano-alumina) and polypropylene fiber
(PPF). Feasibility Comparisons between the different humidity 60%–
98% of at 23 ± 3 C◦ were examined. The strength behavior of alkali
activated mortar with different curing ages was also evaluated. Scanning
electron microscopy (SEM) analysis and X-ray diffractions (XRD) were
also conducted to clarify the effect of nanomaterials and PPF on the
microstructures of AAM. Furthermore, the compressive and flexural
strength at 28 and 90 days of curing were compared to examine the
performance of nano materials and polypropylene fiber (PPF) during a
long curing time.
2. Material
In the current study, locally available low calcium fly ash (FA) from
Euro build and ground granulated blast slag (GGBS) from Chine
confirmed to ASTM C 618 standards [46]. Complementary use GGBS
and fly ash produced more promising performance than alkali-activated
concrete based on fly ash [47], because the mineral composition of the
material is directly related to the development of strength. GGBS and fly
M.H. Dheyaaldin et al.
Fig. 4. AAM specimens under drying shrinkage measurement.
ash include considerable amounts of SiO2, CaO, and Al2O [47]. Table 2
shows the white powdered form of nano SiO2 and nano Al2O3 with
distinct properties that were utilized as additives in the alkali activator
mortar in two different quantities (1% and 2% by weight of binder
materials) with polypropylene fiber (PPF) (0.5%, and 1% percent) by
volume were utilized. Tables 1 and 2 illustrate the chemical composition
of materials analyzed by the X-ray fluorescence (XRF) and physical
properties of binders; nanomaterials and polypropylene fiber (PPF).
Natural sand was utilized as fine aggregates in this investigation, and the
physical properties and sieve analysis of natural sand are shown in
Table 3 and Fig. 1. A combination of sodium silicate (Na2SiO3) and so­
dium hydroxide (NaOH) was utilized as an alkali activator with sodium
silicate to sodium hydroxide ratio 2.5 and the concentration of the NaOH
was 12 M as stated as optimum factors for AAC [17,33,48,49]. The so­
dium silicate (Na2O:17.98%, SiO2: 28.1%, H2O: 53.92% by mass) was
provided by DCP company, Erbil, Iraq. The sodium hydroxide was 98%
pure and flaky in shape was used with a concentration of 12 M which
considered the optimum concentration for AAC [50,51]. Super­
plasticizer (Glenium 51) supplied from Basf company was used to ach­
ieve the optimum workability.
3. Mix design and method
A combination of 50% fly ash (FA) and 50% ground granulated blast
slag by weight were utilized as binder materials for AAM. A constant
binder weight of 700 kg/m3 was used to produce the AAM mixtures and
it is the number of total biner ratio without nanomaterials. In addition of
nano materials by different percentages and it is replaced by weight of
binder. The central composite design (CCD) method was applied to carry
out the mix design using the Design–Expert statistics computer software.
The CCD method was used to assess the individual and synergistic po­
tential effects of three components with three levels on one response.
This method can restrict the number of tests needed to figure out the key
effects and interactions of each variable [52,53]. Nano-silica and
Nano-alumina were used at varied percentages of 1% and 2% of the
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Ceramics International xxx (xxxx) xxx
binder by weight, respectively. Polypropylene fiber (PPF) was added to
the mixture at concentrations of 0.5 and 1% by volume. Tables 4 and 5
displays the mix design materials and weights at kg/m3. It was noted
that the numbers (0-0.5%–1%) indicates polypropylene fiber percent­
ages by volume. The ratio of NS and NA were used was (1% and 2%) by
weight of binder materials [51,54–56]. The dry materials; fine aggre­
gates, fly ash (FA), and ground granulated blast slag (GGBS) were mixed
firstly for 2.5 min then the natural sand was added and mixed for extra
2.5 min. Furthermore; The alkali activator and superplasticizer were
added to the mixture and stirred for an additional 2 min [17,33]. And for
each exact mix, it is three identical specimens were produced.
4. Specimen preparation
The specimen preparation technique of AAM is similar as the spec­
imen preparation technique for cement mortar. The mixing procedure is
starting with 2.5-min mixing of FA; GGBS and nanomaterials then fine
aggregate was added and mixing for extra 2.5 min. The alkali solution
and superplasticizer were added to the mix and mixed for additional 2
min. Finally, the PPF was added to the mix and mixed for additional 3
min with slowly addition of extra water to control the workability of
AAM. The prism (40 × 40 × 160) mm; cubic (50 × 50 × 50) mm and
shrinkage molds were filled with AAM and vibrated gradually with three
layers. The specimens were covered by plastic bag and kept at room
temperature for 24 h (rest period).
5. Curing condition
The specimens were demolded after 24 h and cured at laboratory
(room) temperature for 28 and 90 days to evaluate the compressive and
flexural tensile strength of AAM [57]. Whereas, the prism specimens for
the shrinkage behavior were kept at shrinkage room 23 ± 2 ◦ C and two
various humidity 60%, and 98% humidity as shown in Fig. 2 [58].
6. Length change
The shrinkage comparator is a measurement of length change device
for calculating the shrinkage and expansion strain of AAM as illustrated
in Fig. 4. To cast “mini-bar” prism specimens, a non-standardized mold
with dimensions of (25 mm × 25 mm × 285 mm) was created. Fig. 3
shows the details of the molds was used to measure the drying shrinkage
behavior of AAM under chamber environment. The chambers might
create conditions with varying levels of RH and/or gases (e.g., nitrogen
purge). The mold could be dismantled fully and had a gauge length of
101.6 mm (4 inches). One-inch black oxide alloy steel cone point socket
set screws were utilized as gauge screws. The specimens were placed in
the chambers on a grid panel to allow for uniform drying with no or little
restraint according to the ASTM C490/C490M standard [59]. The
measuring instrument must have an accuracy of 0.002 mm in any 0.026
mm range and 0.005 mm in any 0.25 mm range, as well as a sufficient
range (at least 7.62 mm) to account the average differences in the actual
length of various specimens. For the first three weeks, measurements
were taken every 24 h, and subsequently three times a week. Weight loss
measures were also taken on the same specimens at the same time. AAM
free shrinkage measurements were taken on four prism specimens for
each mix.
7. Compressive and flexural tensile strength
The cubic molds (50 × 50 × 50 mm) and prism molds (40 × 40 ×
160 mm) were used to evaluate the compressive and flexural tensile
strength test respectively [60]. The specimens were kept at room tem­
perature for 24 h. The specimen was cured at ambient conditions for 28
and 90 days. Three identical specimens were tested for compressive and
flexural tensile strength according to ASTM C109 [61] and British
standard BS EN 196-1:2005 [62] respectively. Fig. 5 shows the molds
M.H. Dheyaaldin et al. Ceramics International xxx (xxxx) xxx

Fig. 5. (a) Cubic mold (50 × 50 × 50). (b) Prism mold (40 × 40 × 160) mm. (c) Flexural tensile strength test machine. (d) Compressive strength test machine.

Fig. 6. Drying shrinkage values of AAM at 60% RH. Fig. 7. Expansion of AAM at 98% RH.

6
M.H. Dheyaaldin et al.
Fig. 8. Compressive strength of alkali activated mortar at 28- and 90-days.
Fig. 9. Flexural tensile strength of alkali activated mortar at age of 28- and
90-days.
and machines used to measure the compressive and flexural tensile
strength.
8. Result and discussion
8.1. Length change of geopolymer mortar
8.1.1. Length change of AAM at 60% humidity
The drying shrinkage of AAM specimens was tested for 60 days.
Fig. 6 illustrates the length variation of the alkali activated mortar. It
was shown that the length of AAM has been decreased, and shrinking
began at an early age and has increased with time. Compared to other
mixes, the dry shrinkage of alkali activated mortar for control specimens
(specimens without nanomaterials and PPF) is the highest. The inclusion
of nano alumina (NA) and nano-silica (NS) improved AAM shrinking.
The use of NS and/or NA alone, on the other hand, had a lower influence
on the shrinking behavior of AAM compared to the combined effect and/
or the fibrous mixes (mixes include PPF fibers). NS had a somewhat
better effect than NA. The combination of NS and NA had a substantial
influence on AAM shrinking behavior. Furthermore, polypropylene fiber
significantly improved the shrinkage behavior of AAM; AAM containing
0.5% PPF exhibited lower shrinkage values than AAM containing 1%
PPF. However, the use of PPF with NS and/or NA resulted in the smallest
amount of shrinkage of AAM with superior improvements. Shrinkage
values for AAM specimens containing 0.5% PPF ranged from 280 to 360
micro strains, whereas specimens containing 1% PPF ranged from 360 to
450 micro strains. The shrinkage value for specimens including both NA
and NS with and without PPF was 300–340 micro strain. Furthermore,
AAM containing NA and/or NS with 0.5% PPF showed decreased
7
Ceramics International xxx (xxxx) xxx
shrinkage values ranging from 280 to 310 micro strain.
The incorporation of polypropylene (PPF) was shown to successfully
minimize the drying shrinkage of regular cement mortar sample [63].
The shrinkage of ordinary cement mortar increases as the amount of
nano-silica increases [64]. It was indicated that the addition of 1% and
2% of nano-silica was increased the shrinkage by 93.7%, especially at
the early days of cement hydration (3 days). Nano-silica with the high
pozzolanic activity can play a significant role in early ages, resulting a
higher degree of cement hydration and resulting in the promotion of
higher shrinkage [64].
8.1.2. Length change of AAM at 98% humidity
The length changes of AAM with the humidity of curing condition
changes. The length of specimens was expanded at the condition 98%
humidity and 24 ± 4 ◦ C (room temperature). Fig. 7 illustrated the length
rate of AAM specimens; it was noted that the length of specimens was
changed and expanded. The inclusion of nano-materials and/or the
addition of polypropylene fiber (PPF) has a substantial effect on the
length change of AAM. The expansion of AAM was marginally reduced
compared to specimens without polypropylene fiber (PPF) and/or nano-
materials. The ratio of fibers and/or nano-material even showed
improvement and reducing the length’s expansion. The combined use of
0.5% PPF with both nano-materials had better improvement than
specimens contain 1% PPF and nano-materials. Specimens contain 2%
nano alumina (NA), 1% nano silica (NS) and 0.5% polypropylene fiber
(PPF) exhibit lowest expansion.
8.2. Mechanical properties
8.2.1. Compressive strength
It has also been discovered that the addition of nano-Al2O3 particles
to cement-based composites improves the strength of C–S–H gel for­
mation and strengthens the interfacial transition zone of cement-based
specimens [65]. The compressive strength of alkali activated mortar is
also increasing due to curing ages, Fig. 8 demonstrated the compressive
strength of alkali activated mortar at ambient room temperature at 28
and 90 ages. The specimens contain 2% nano-alumina (NA) exhibits 82
MPa at 28 days, and 89.9 MPa at 90 days at ambient temperature. It is
slightly increasing and has a superior result when compared to other
mixes, and the specimens contain 0.5% polypropylene fiber (PPF); 1%
nano-silica (NS), and 1% nano-alumina (NA) have a lower compressive
strength at 90 days when compared to 28 days ambient curing. Speci­
mens containing 1% nano-silica (NS) and 1% nano-alumina (NA) pro­
duced about 87.3, with a considerable improvement in strength after 90
days. Dheyaaldin et al. [18] studied the performance of AAM at ambient
environment at 7 and 28 days. They founded also the combination of 1%
of nano alumina (NA), 1% nano silica (NS), and 0.5% of polypropylene
fiber (PPF) exhibited the lowest compressive strength. The combined use
of 2% for both nanomaterials had a negative impact on compressive
strength results compared to mixes containing NS and NA alone. The use
of 2% nano-silica and nano-alumina alone, on the other hand, had a
significant influence on the compressive strength of AAM and signifi­
cantly enhanced it [18]. The polypropylene fiber (PPF) in the AAM
specimens increased the strength of the mortar, but as compared to the
specimens containing nano materials, the strength was lower.
Nano-alumina has a greater influence on the mechanical and material
characteristics of hardened AAM than nano-silica [66]. The compressive
strength of alkali activated mortar increased significantly as the reac­
tivity of the alkali activated matrix product increased. The alkali acti­
vated’s strength increases with the addition of nano silica, and it can
have the structure of C–S–H, C–A–S–H, or N–A–S–H gel. It’s most likely
due to the large number of fibers influencing the alkali activated reac­
tion and introducing additional interfaces [67].
8.2.2. Flexural strength
According to previous study, the incorporation of polypropylene
M.H. Dheyaaldin et al.
Fig. 10. SEM-photographs of AAM specimens.
fiber (PPF) improved the flexural tensile strength, and shrinkage
reduction. It is thought that the incorporation of 1% PPF improves the
flexural tensile strength performance to its maximum potential [26].
Dheyaaldin et al. [18] studied the flexural tensile strength of AAM at 7
days 28 days, AAM mixes containing 1% polypropylene fiber (PPF) had
lower flexural tensile strength than the control mix, but at 28 days, it had
higher flexural tensile strength, demonstrating that polypropylene fiber
(PPF) provides flexural tensile strength improvement as a function of
age. Flexural tensile strength was reduced in mixtures containing 1%
nano silica and 1% nano alumina compared to the mixes containing
either nano silica or nano alumina separately [18]. The flexural tensile
strength of alkali activated mortar shown in Fig. 9. High flexural
strength at ambient curing temperature at 28 and 90 days was achieved
8
Ceramics International xxx (xxxx) xxx
through the combined use of nanomaterials and PPF fibers; the speci­
mens containing PPF have catches bonds between materials and fiber,
and the specimens containing 1% NS and 1% PPF show better perfor­
mance and highest flexural strength, which is approximately 22.2 MPa
at 90 days, compared to specimens containing 0.5% PPF. On the other
hand, specimens with 0.5% PPF at 28 curing days achieve higher flex­
ural tensile strength.
The performance of nano materials alone on the flexural tensile
strength is not significant when compared to PPF specimens, and the
strength of AAM is somewhat lowering, especially when specimens
include nano materials separately. However, specimens include 1% NA,
and 1% NA has been increasing at age of 90 days compared to the
control specimens (without nanomaterials).
M.H. Dheyaaldin et al.
Fig. 10. (continued).
8.3. Microstructure analysis
8.3.1. Scanning electronic microscopy (SEM)
Scanning electronic Microscopy (SEM) were taken for the specimens
includes (2% NA; 2% NS and 2% NA; 1% NA-1% PPF, 1% PPF; 1% NS;
2% NA and 0.5% of PPF, 1% NS, 1% NA and 0.5% of PPF) and shown in
Fig. 10. Generally, the AAM specimens had different microstructures
depending on the ratio of materials, and curing conditions.
Specimens includes 2% of nano-alumina performed an act as fillers
by filling pores spaces and improved filler particles between binder
phase (FA and GGBFS). The AAM matrix is expected to have a big impact
on the material’s overall strength. As a result, this cohesion appears to
9
Ceramics International xxx (xxxx) xxx
strengthen the relationship between reactive and pore spaces in SEM
capture, where capillary holes expand with the addition of nano-
alumina. Alumina nanoparticles, on the other hand, appear to act as a
filler in the binder structure, working to create a denser structure by
lingering in the voids, although they may obstruct the development of
C–S–H, which has yet to be found. Only a small amount of gel forms
since the majority of the fly ash and slag is left unreacted [68].
Regardless of the solution-to-binder ratio of the AA mortar, SEM
showed that the mortar produced a comparably dense reactive product.
Cracks in the AAM gel were hypothesized to have formed during
compressive strength testing or when the specimen was stored in various
relative humidity conditions for SEM. In this study, the compacted
M.H. Dheyaaldin et al.
Fig. 10. (continued).
structure of mortar indicated that there was a considerable amount of
reacted product, indicating strong compressive strength. This might be
due to the effects of nano-alumina filling the gaps to form denser AAM,
or it could be due to the higher quantities of AAM gel and amorphous
components in the NA-geopolymer specimens filling the system’s micro-
level voids [44].
Fig. 6 indicates that specimens include both nanomaterials and 0.5%
PPF. The combination of fibers and nanomaterials resulted in a high
degree of bonding, as well as the lack of apparent deformation on the
fiber surface, which is a desired characteristic in terms of specimen
length and long-term properties (I, j, k, and L). All of the fibers
demonstrated a significant improvement in drying shrinkage results
10
Ceramics International xxx (xxxx) xxx
when compared to the control specimen. After being exposed to air for
21 days, all of the fiber reinforced AAM composites had drying
shrinkage values less than 400 microstrains, and the fibers displayed a
constant rate of drying shrinkage after 21 days. The presence of fibers
results in a high degree of bonding and no noticeable deformation on the
fiber surface, both of which are desirable qualities in terms of durability
and long-term performance similar to the results shown in study con­
ducted by Al-Mashhadani et al. [63].
8.3.2. X-ray diffractions (XRD)
AAM nanocomposites have a higher flexural tensile strength due to
the improved pore filling mechanisms. When Nano-Al2O3 is dispersed
M.H. Dheyaaldin et al. Ceramics International xxx (xxxx) xxx

crystalline composite in AAM matrices [50,70]. Peak positions were

noticeable in the XRD analysis of alkali activated mortar with a 2% NS
addition, as they were in the specimens containing nano-silica. The
crystalline quartz was found in the 20◦ –27◦ 2 h region as a result of the
formation of crystalline composite in AAM matrix.
XRD patterns of PPF with and without nano-Al2O3, nano-SiO2
composed of the crystallized phases of quartz and Al(PO3) with amor­
phous hump to degree of 21◦ –29◦ , is thought to form as a by-product of
the formation of an aluminosilicate gel in geopolymeric systems, con­
cerning pattern comparison, and explained that XRD of geopolymer of
recent study for the specimens includes PPF are also similar to other
specimen.

9. Conclusion

In this research, the length change of alkali activated mortar of hu­

midity curing room has been studied, as well as the strength of geo­
polymer was considered and calculated. And the strength and length
change performed by using waste PP fibers and nanomaterials such as
nano-silica SiO2 and nano alumina Al2O3, were investigated and the
following conclusions are summarized:

• The influence of NA; NS and PPF on the compressive strength of AAM

Fig. 11. XRD analysis of alkali activated mortar.
uniformly throughout the matrix, it fills voids and creates a denser
microstructure [69]. The XRD patterns of AAM include nano-Al2O3, fly
ash/ggbs, and nano-silica-are shown in Fig. 11(a). The presence of
crystalline phases of quartz in fly ash and ggbs binders with an amor­
phous hump between 20.5◦ and 26◦ is connected to the production of an
alumino-silicate gel in geopolymeric systems. The XRD analysis of the
reference mortar, AAM without NS, and AAM with 6% NS was per­
formed. A couple of additional peak locations were visible in the XRD
picture for alkali activated mortar with a 6% NS addition. Crystalline
quartz was identified in the 26–32◦ 2 h region due to the production of
was very low; the compressive strength of alkali activated mortar
increased throughout curing ages, whereas specimens containing 2%
NA performed stronger than specimens containing PPF; also, speci­
mens containing 1% NA, 1% NS performed stronger than specimens
containing 2% NS and roughly less than 2% NA.
• The flexural tensile strength of AAM containing PPF increases with
curing time, the specimens containing PPF have catches bonds be­
tween materials and fiber, and the specimens containing 1% NS and
1% PPF show better performance and the highest flexural strength,
which is approximately 22.2 MPa at 90 days, compared to specimens
containing 0.5% PPF.
• The performance of nano materials on flexural tensile strength is not
significant when compared to PPF, and the strength of AAM is
somewhat lowering, especially when specimens include nano mate­
rials separately. However, specimens include 1% NA, and 1% NA has
been growing at 90 days.
• The length of alkali activated mortar decreasing and it is shrinkage of
60% humidity in 24 + 2 C room temperature. The specimens contain
PPF has better performance on change of geopolymer length
compared to specimens without PPF fiber and specimens contain
nano materials shrinkage compared to control specimens, but read
more shrinkage than PPF, by all mean that the PPF is reduced
shrinkage of alkali mortar of 60% humidity and 0.5% PPF fiber was
performed better performance than 1% PPF with nano materials and
specimens contain 2% NA was performed higher shrinkage
compared to control specimen without nano materials and PPF.
• The change length of 98% humidity at 24 + 2 C room temperature
has been expanded, and it was considered on additive on geopolymer
mixes, and illustrated that specimens contain PPF is controlling the
expansion of alkali mortar and the best result and less expanded
mortar contain 0.5% PPF and nano materials compared to specimens
without PPF gives higher expanded on geopolymer length.
• This research conducted that the effect of humidity percentage has
significant role on geopolymer length, and the PPF shows better
performance of 60% and 98% room humidity.
• Specimens includes 2% of nano-alumina performed an act as fillers
by filling pores spaces and improved filler particles between binder
phase (FA and GGBFS). The AAM matrix is predicted to have a
considerable impact on the material’s overall strength. As a result,
this cohesion appears to strengthen the relationship between reactive
and pore spaces in SEM capture, where capillary holes expand with
the addition of nano-alumina.

11
M.H. Dheyaaldin et al.
• Alumina nanoparticles, on either side, appear to operate as a filler in
the binder structure, persisting in the spaces to help produce a denser
structure, however they may inhibit the development of C–S–H,
which has yet to be discovered. Only a small amount of gel forms
since the majority of the fly ash and slag is left unreacted.
• AAM nanocomposites have a higher flexural tensile strength due to
the improved pore filling mechanisms. When Nano-Al2O3 is
dispersed uniformly throughout the matrix, it fills voids and creates a
denser microstructure.
• The mechanical characteristics of AAM are intimately connected to
the formation of micro-cracks and the bonding between poly­
propylene (PPF) and the AAM matrix.
• While the trends in XRD patterns of AAM pastes containing nano-
Al2O3 and both together are comparable to those in nano-SiO2 and
both together, the phases are vastly different. Because these phases
are not included in the geopolymeric synthesis, AAM contains these
filler particles. Specimens includes Polypropylene fiber, like other
specimens, has varying ratios of nanomaterial, and the crystalliza­
tion of quartz and Al (PO3) phases is extremely different.
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.
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