Case Studies in Construction Materials 15 (2021) e00737

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Case Studies in Construction Materials

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Fabrication of thermal insulation geopolymer bricks using

ferrosilicon slag and alumina waste
M.M. Ahmed a, 1, K.A.M. El-Naggar b, 1, Dalia Tarek c, 1, Ayman Ragab c,
Hesham Sameh d, Abdullah M. Zeyad e, f, Bassam A. Tayeh g, *, Ibrahim M. Maafa h,
Ayman Yousef a, h, *
a
Department of Mathematics and Physics Engineering, Faculty of Engineering at Mataria, Helwan University, Cairo 11718, Egypt
b
Department of Chemical Engineering, Egyptian Academy for Engineering and Advanced Technology, Cairo, Egypt
c
Department of Architecture Engineering, Faculty of Engineering, Aswan University, Aswan, Egypt
d
Department of Architecture Engineering, Faculty of Engineering, Cairo University, Cairo, Egypt
e
Department of Civil Engineering, Faculty of Engineering, Jazan University, Jazan 11451, Saudi Arabia
f
Department of Civil Engineering, Faculty of Engineering, University of Science and Technology, Aden, Yemen
g
Civil Engineering Department, Faculty of Engineering, Islamic University of Gaza, P.O. Box 108, Gaza Strip, Palestine
h
Department of Chemical Engineering, Faculty of Engineering, Jazan University, Jazan 45142, Saudi Arabia

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

Keywords: The present study introduces the preparation of thermal insulation geopolymer bricks using
Ferrosilicon slag ferrosilicon slag and alumina waste. Compressive strength, bulk density, cold and boiling water
Alumina waste absorption, apparent porosity, thermal conductivity, and Fourier-transform infrared spectroscopy
Bricks
were used to characterized the geopolymer bricks. Ferrosilicon slag suffers from low alumina
Geopolymer
Compressive strength
content. Thus, alumina is added to compensate for this deficiency. Pristine ferrosilicon slag and
Thermal conductivity the SiO2/Al2O3 (Si/Al, ratio = 2) sample were prepared at different NaOH concentrations (i.e., 6,
8, 10, and 12 M; Na2SiO3/NaOH ratio = 2.5), different curing times (i.e., 3, 7, 14, and 28 days),
and room temperature. The 8 M NaOH concentration achieved the best compressive strength.
Accordingly, different Si/Al ratios were prepared and tested at 8 M NaOH, room temperature, and
different curing times (i.e., 3, 7, 14, and 28 days). Results indicate that increasing the alumina
content enhances the geopolymer properties but reduces the compressive strength of the prepared
geopolymer. The sample with Si/Al ratio = 1 exhibited a higher compressive strength (10.9 MPa)
than the other Si/Al ratios (i.e., 4, 3, 2, and 0.5) and the pristine ferrosilicon slag after 28 days of
curing and at 8 M NaOH. The obtained value is consistent with the ASTM C62 and Egyptian
standards. Furthermore, the addition of alumina waste decreased the thermal conductivity of the
prepared geopolymer bricks.

1. Introduction

Energy consumption in the production of fired bricks is extremely high due to the high production temperature (900–1000 ◦ C) in
kiln firing, which is accompanied by massive greenhouse gas emissions (e.g., CO2 and NOx emissions) [1–4]. Bricks production mostly

* Corresponding authors.
E-mail addresses: btayeh@iugaza.edu.ps (B.A. Tayeh), aymanyousef@m-eng.helwan.edu.eg (A. Yousef).
1
The authors have the same contribution in the first author.

https://doi.org/10.1016/j.cscm.2021.e00737
Received 21 July 2021; Received in revised form 23 September 2021; Accepted 8 October 2021
Available online 11 October 2021
2214-5095/© 2021 The Author(s). Published by Elsevier Ltd. This is an open access article under the CC BY-NC-ND license
(http://creativecommons.org/licenses/by-nc-nd/4.0/).
M.M. Ahmed et al. Case Studies in Construction Materials 15 (2021) e00737

uses clay and shale as raw materials, which are not considered eco-friendly and economical due to the high energy required and the
consumption of natural resources [5–8]. Thus, the exploration of alternative construction materials to address the aforementioned
issues has received increasing attention in recent years. In the addition to insufficient landfill spaces, industries are known to discharge
huge amounts of waste materials, which are economic and environmental issues [9–15]. The use of waste materials in building bricks
production could mitigate the landfilling issues and reduce the consumption of natural resources and their quarrying operation costs
[16]. Furthermore, this approach helps in reducing the energy requirement by avoiding burning or high efforts needs to do waste
disposal and their better utilization. Researchers have utilized a wide variety of waste materials (e.g., fly ash, slags, mine tailings, rice
husk ash, cotton waste, oyster-shell, and wood sawdust) in brick production as a replacement or an additive [1,17–30]. Geo­
polymerization technology has been introduced as an alternative route for bricks production using various wastes from industrial
by-products composed of rich aluminosilicate materials due to the environmental and economic benefits of recycling wastes [31,32].
This process involves the chemical reaction between the aluminosilicate materials from industrial by-products and a highly concen­
trated aqueous alkali hydroxide or silicate solution, which produces a very stable material with an amorphous polymeric structure
[1–6]. During the reaction, the geopolymer gel network forms the sodium aluminosilicate hydrate gel (N-A-S-H). N-A-S-H has a
tetrahedral network of SiO4 and AlO4 with shared oxygen atoms, resulting in a three-dimensional structure [32,33]. Accordingly, an
appropriate silica to alumina ratio must be maintained to produce a geopolymer. The concentration of alkali solution is very important
for the formation of the geopolymer network of N-A-S-H. Several of the previous studies in multi-use concentration of sodium hy­
droxide molarity solution of 6 M, 8 M, 10 M and 12 M [34–38]. Many geopolymer starting materials are deficient in aluminosilicate;
thus, additional materials are required to improve the physical and mechanical properties of geopolymers or prepared geopolymers
pastes with a low SiO2/Al2O3 (Si/Al) molar ratio [39]. This ratio produces a geopolymer with large surface area, which is beneficial to
the adsorption capacity [40,41]. Suchanya Apithanyasai et al. [32] fabricated geopolymer bricks for pavement applications from a
mixture of fly ash, electric arc furnace slag, and waste foundry sand, which is the main material composition. However, waste foundry
sand has low alumina and calcium contents, requiring the addition of different proportions of fly ash and electric arc furnace slag to
improve the alumina and calcium ratios and subsequently improve the compressive strength. In the same manner, a secondary source
of alumina is used to prepare a rice husk ash (RHA)-based geopolymer with improved properties [2,42–46]. Alumina sources can be
used to compensate for the shortcomings of RHA [44,45]. Ehsan Mohseni et al. [47] added nano-Al2O3 to RHA to prepare a RHA-based
geopolymer, compensating for the Al2O3 deficiency of RHA. The mechanical properties also improved due to the formation of calcium
silicate hydrate (C-S-H) or calcium aluminosilicate hydrate (C-A-S-H) and sodium aluminosilicate hydrate (N-A-S-H) or a geopolymer
gel in the alkali-activated matrix. Thus, alumina must be added low-alumina materials [47]. Ferrosilicon slag (FS) is a by-product
material of silicon and ferrosilicon industries after reducing high-purity quartz using coal in an electric arc furnace. Thus, it has a

Fig. 1. Slag materials before and after grinded, (a): FS befor grinded, (b): AW befor grinded, (c): FS after grinded, (d): AW after grinded.

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M.M. Ahmed et al. Case Studies in Construction Materials 15 (2021) e00737

high amount of free silicon, which might be discharged with the slag. Given its low cost, it is used in steel-making and Portland cement
industries. Under alkali condition, free silicon is oxidized by H2O, releasing H2 gas, which leads to the formation of geopolymer foams
[48,49]. Geopolymer foams are prepared at low temperature (< 100 ◦ C) and exhibit characteristics similar to glass or ceramic foams,
which are fabricated at high temperature (> 900 ◦ C) [48,50]. In addition, geopolymers tiles can be used as an alternative to ceramic
materials, which are usually obtained by calcination of clay at high temperatures (900–1000 ◦ C) [51–53]. Geopolymer foams are used
in high-temperature applications (e.g., like fire resistant coatings, thermal insulation, and wall panels) [48,54,55]. These foams mostly
have a light-weight structure and thus appropriate for thermo acoustic insulating and fire resisting applications [48,56]. However, FS
is deficient in Al2O3, thus, an alumina source is needed to compensate this deficiency in order to achieve the reaction between Si/Al in
the presence of alkaline solution to produce a geopolymer gel (N-A-S-H). A large amount of alumina waste (AW) is produced after
quenching smelt aluminum. This slag is a costless material and can thus be used to compensate for the Al2O3 deficiency of FS. AW is a
cost-effective material and exhibits superior performance as a building material [57]. AW has many advantages, including high
refractoriness, high compressive strength and hardness, good chemical purity, and excellent thermal stability and shock properties
[58]. Furthermore, AW can also improve the fire resistance for high-temperature applications [59,60]. According to the World Bureau
of metal statistics, the annual production of aluminum in Egypt is approximately 258,000 tons [61,62]. Few studies have used alumina
in the preparation of geopolymer composites to compensate for the alumina deficiency of materials to improve the geopolymer
properties [39,47,57,63]. According to previous literature, there is a paucity in previous research or studies that indicate the use of FS
in the production of cement or geopolymer concrete as a supplemental material or basic. In addition to the lack of previous studies on
the use of FS and AW in the production of lightweight geopolymer concrete or geopolymer-based thermal insulating bricks. Hence the
importance of this experimental study for the use of FS in the manufacture of geopolymer bricks through the production of lightweight
thermal insulation bricks. This research will open the horizon and encourage the use of industrial waste from FS in the construction
industry within cement concrete or geopolymer. Thus, bricks were prepared in this study for non-load bearing. The compressive
strength, density, water absorption, porosity, thermal conductivity, Fourier-transform infrared spectroscopy (FTIR) images, scanning
electron microscopy (SEM) images, and water absorption of the samples were examined. The sample with high alumina exhibited a
high compressive strength. The results of this study can be used to create environmentally friendly solutions for industrial waste
management. Fig. 1 shows the schematic of the production of thermal-insulating geopolymer bricks from industrial waste in this study.

2. Experimental

2.1. Materials and methods

The ferrosilicon slag (FS) material was purchased from an Egyptian ferrosilicon company, Edfou, Aswan, Egypt. The aluminum slag
(alumina waste, (AW)) material was purchased from an Egyptian aluminum company, Nag Hammadi, Qena, Egypt.

2.2. Preparation of slag powder

The large size slag particles was collected from the landfill of factories (Fig. 1). Slag is grinded to obtain fine particles, which it goes
through several stages. (1) the crushing stage is done by placing peat in the crushing machine to turn it into small granules with an
average diameter of 2 mm. (2) the smoothing stage, in which a ball mill is used, uses a steel container with a volume of 20 liters and a
rotational speed of 90–110 revolutions per minute. Balls of various diameters (1,2, 3 and 4 cm) are placed with 20 balls for each
diameter. The grinding process is continuous for 4 h. Finally, fine powder is obtained (Table 1).

2.3. Composition of FS and AW

Table 2 shows the chemical analysis of FS and AW through X-ray fluorescence (XRF). Prior to XRF analysis, the slag materials were
ground using a ball mill to reduce their particle sizes. Sodium hydroxide (NaOH, 98%) pellets and a sodium silicate (Na2SiO3, 30.1%
SiO2, 9.4% Na2O, and 60.5% H2O, with silicate modulus SiO2/Na2O = 3.2, and specific gravity = 1.5 g/ml at 20 ◦ C) solution were
purchased from Fisher Scientific, UK.

2.4. Characterization

The FS and AW compositions were determined through XRF (MXF 2400 Shimadzu) and XRD (Rigaku Co., Japan, wavelength at
1.54056 Å for Cu Kα radiation). The morphology and mineral phase compositions of the selected prepared geopolymer foam samples
were identified by SEM (Hitachi S-7400, Japan) and XRD, respectively. The composition or function groups of the starting materials

Table 1
Physical properties of FS and AW.
Physical properties Specific Specific Color
gravity area (cm2/gm)

FS 2.56 12,050 Hard Gray

AW 2.51 11,910 Light Gray

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M.M. Ahmed et al. Case Studies in Construction Materials 15 (2021) e00737

Table 2
Chemical composition of FS and AW.
Chemical SiO2 Al2O3 Fe2O3 CaO MgO TiO2 Na2O K2O P2O5 SO3 Cl LOI
composition
(%)

FS 77.70 3.45 11.50 1.96 0.14 0.11 0.26 0.35 0.07 0.39 0.06 3.85
AW 2.62 64.5 0.46 0.47 8.31 0.13 4.29 3.61 – 0.42 9.82 2.74

and the prepared geopolymer foams were also confirmed using a FTIR spectrometer (Bruker-Optic Tensor 27, Germany). The obtained
FTIR graphs were scanned within a wavenumber range of 400–4000 cm− 1. Three different foamed geopolymer samples for each
composition batch were selected to determine the bulk density, the apparent porosity, the water absorption, and the compressive
strength according to [ASTM C20] and [ASTM C109]. The compressive strength was determined using an automatic hydraulic testing
machine of type ELE with a maximum capacity of 1000 KN at 0.025 N/mm2/s. The compressive strength of the geopolymers was
measured after different curing ages (3, 7, 14, and 28 days). The thermal conductivity of the foamed geopolymer samples was
determined using a KD2 Pro Thermal Properties Analyzer, which uses a transient heat conduction algorithm to digitally record the
thermal conductivity at room temperature.
Fig. 2 shows the XRD analysis of FS powder. The XRD analysis in Table 3 shows that the FS contains silicon within the chemical
formula (Si), and the quartz, low-alpha phase (SiO2) of the mineral composition of the slag. In addition, FS containing the ferdisilicite
(FeSi2). The use of this type of slag as pore agent for the production of air bubbles inside the matrix of geopolymer for the production of
thermal insulation geopolymer bricks. As the presence of metals in the slag composition used as pore agent.
Fig. 3 displays the XRD patterns of the AW, as shown in the Table 4, the evident of diffraction peaks mainly hexagonal alumina with
significant amount of rhombohedral corundum, cryolite (Na3 Al F6), Viitaniemiite (Na Al (PO4) (Fe OH)3), and goethite (FeO OH).

2.5. Alkaline activator preparation

The NaOH pellets (99% purity) were dissolved in the distillated water to prepare of 6, 8, 10, and 12 M aqueous NaOH solutions. The
prepared solutions were left to cool down to room temperature. The alkaline solution was a mixture of the aqueous solutions of NaOH
and Na2SiO3. The different aqueous NaOH solution concentrations were mixed separately with a Na2SiO3 solution to finally obtain the
alkaline activator (Na2SiO3/NaOH) ratio of 2.5. This ratio was maintained in all the experiments. The solution was prepared 24 h
before use.

2.6. Sample preparation

The precursor materials for fabricating geopolymer bricks were mixed according to the mix proportions shown in Table 5. The
powder was pre-mixed for 10 min according to the proportions provided in Table 5. Then, the alkaline solution was slowly added to the
powder mixture. The SA denoted the mixture from FS and AW. The SA-3 samples were mixed with alkaline solutions of different NaOH
concentrations (i.e., 6, 8, 10, 12 M). The solid/liquid ratio was 4:1 to obtain good workability. The fresh geopolymer slurries were
rapidly cast into PVC cube molds (50 cm × 50 cm × 50 cm) and left for 24 h at room temperature before demolding. This mold size
was adopted to decrease the consumption of raw materials. The compressive strength of the geopolymer foam samples was tested after
3, 7, 14, and 28 days of curing and storage at room temperature. The sample with 8 M NaOH demonstrated the highest compressive
strength. Thus, this solution was used to prepare the other formulations with different (Si/Al) ratios (Table 1), following the

Fig. 2. XRD analysis of FS.

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M.M. Ahmed et al. Case Studies in Construction Materials 15 (2021) e00737

Table 3
Mineral composition of FS.
Ref. Code % Compound name Chemical formula

00-026-1481 54.25 Silicon Si

00-039-1425 6.25 Cristobalite SiO2
00-005-0490 25.42 Quartz, low-alpha SiO2
00-035-0822 12.51 Ferdisilicite FeSi2

Fig. 3. XRD analysis of aluminum slag.

Table 4
Mineral composition of aluminum slag.
Ref. Code % Compound name Chemical formula

01-078-5519 48.9 Hexagonal alumina Al2O3

01-075-0782 21.20 Rhombohedral corundum Al2O3
01-082-0216 6.24 Cryolite Na3(AlF6)
00-035-0598 15.55 Viitaniemiite Na Al (PO4) (Fe OH)3
01-081-0462 9.25 Goethite Fe O(OH)

Table 5
Composition of prepared brick geopolymer foams (mixture (100 g)).
Samples SiO2 Al2O3 Na2O H2O Alkaline activator Si/Al NaOH Alkaline activator ratio
(g) (g) (g) (g) (g) (Molar) (Na2SiO3/NaOH)

FS-6 62.16 2.76 2.38 13.52 20 22.5 6 2.5

FS-8 62.16 2.76 2.62 13.28 20 22.5 8 2.5
FS-10 62.16 2.76 2.84 13.06 20 22.5 10 2.5
FS-12 62.16 2.76 3.05 12.85 20 22.5 12 2.5
SA-1-8 54.45 12.53 3.27 13.28 20 4.3 8 2.5
SA-2-8 51.44 14.97 3.43 13.28 20 3.4 8 2.5
SA-4-8 36.43 31.48 4.23 13.28 20 1.15 8 2.5
SA-5-8 26.42 35.32 4.79 13.28 20 0.75 8 2.5
SA-3-6 46.44 19.03 3.45 13.52 20 2.4 6 2.5
SA-3-8 46.44 19.03 3.69 13.28 20 2.4 8 2.5
SA-3-10 46.44 19.03 3.91 13.06 20 2.4 10 2.5

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M.M. Ahmed et al. Case Studies in Construction Materials 15 (2021) e00737

aforementioned procedures of preparation and tests. The SA-4 sample exhibited the highest compressive strength. After the
compressive strength test, the remaining geopolymer fragments were ground and kept for XRD, SEM, and FTIR analyses.

3. Results and discussions

3.1. Particle size distribution of raw materials

Fig. 4 shows the particle size distribution of both raw materials, the FS and AW. It seems that the AW material is finer than that of
the FS as evidenced by the differences in their median sizes (D50). The mean particle size for the FS and AW is 1.35 µm and 2.4 µm,
respectively. This inconsistency in sizes will assist in particles of AW placing themselves between those of FS, which could be reducing
the porosity of the mixture.

3.2. Compressive strength

The compressive strength of FS was tested at different NaOH concentrations (6–12 M). Fig. 5 shows the compressive strength
results. The appropriate sodium hydroxide concentration based on the literature ranges from 5 M to 15 M [1,18,23,24,26,29]. The
compressive strength increased for the prepared samples with the NaOH concentration up to 8 M in all curing ages. This result can be
attributed to the increased Na2O content in the mixture that enhanced the dissolution of Si and Al species, promoting geopolymeric gel
formation [64]. However, the low alkalinity (i.e., low Na2O) did not provide sufficient hydroxyl groups (OH-) to dissolve Si and Al,
demonstrating low strength. Increasing the alkalinity above 8 M NaOH reduced the strength. This phenomenon may be due to the
rapid and high dissolution of the aluminosilicate species, resulting in the crystallization of aluminosilicate gels at the early stages and
insufficient compaction of specimens, which have a negative impact on the compressive strength of the bricks [1]. The increase in Si/Al
ratio to more than three times formed the low-compressive-strength two-dimensional cross-linked polysialate, while the Si/Al ratio
from 1.5 to 2 produced a three-dimensional network [65]. Thus, SA-3 exhibited a better compressive strength than the sample FS at
different NaOH concentrations (8–12 M). This result could be due to the addition of alumina to FS to improve the Si/Al ratio. The
maximum compressive strength was obtained at 8 M. Furthermore, an increase in compressive strength was observed with the
increasing curing age. Hence, the low compressive strength of FS may be due to its low alumina content. The high silica content led to a
decrease in strength, which is linked to the amount of unreacted materials in the specimens, which act as defect sites [66]. In SA-3,
alumina reacted with the alkaline solution and produced a significant amount of [Al(OH)4]-, which can enhance the geo­
polymerization reaction properties [39]. Kouamo et al. [39] indicated that the compressive strength of volcanic ash improved by
32.4% with the addition of 40%, which compensated for the shortage in ash. Fig. 5 C shows the effect of Si/Al proportion on the
compressive strength results after 3, 7, 14, and 28 days of curing and with 8 M NaOH. Fig. 5 indicates the positive effect of AW on the
compressive strength of geopolymer brick foams from increasing the curing ages at room temperature. The compressive strength of the
geopolymer bricks increased with the alumina content. The SA-4-8 sample displayed the highest compressive strength, obtaining
10.89 MPa after 28 days of curing, which is in accordance with the 10.3 and 8.6 MPa of the ASTM C62 and Egyptian standards,
respectively [67]. Ehsan et al. [47] fabricated lightweight geopolymer composites using RHA, nano-alumina, scoria particles, and
polypropylene. They added nano-alumina to compensate for the shortage of alumina in RHA. The addition of nano-alumina (20%) to
the mixture could improve the mechanical properties due to the formation of calcium aluminosilicate hydrate (C-A-S-H) and sodium
aluminosilicate hydrate (N-A-S-H) or geopolymer gel in the alkali-activated matrix [68]. The increase in the addition of scoria (0–20%)
lead to the decrease in compressive strength and density. Tanakorn et al. [63] added nano-alumina (0, 1, 2, 3 wt%) to calcium fly ash
geopolymer paste, reducing the setting time. Furthermore, the increase of the compressive strength from 39.4 MPa to 56.4 MPa with
the addition of 2 wt% of nano-alumina could be due to the formation of additional reaction products, C-A-S-H and N-A-S-H gels, in the

Fig. 4. Particle size distribution of slag materials after grinded, (a): Particle sizes distribution of FS, (b): Particle sizes distribution of AW.

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M.M. Ahmed et al. Case Studies in Construction Materials 15 (2021) e00737

Compressive strtength (MPa)

6

0
FS-6 FS-8 FS-10 FS-12
3-days 3.8 5.2 4.18 4.88
7-days 3.86 5.33 4.39 5.12
14-days 3.92 5.92 4.46 5.19
28-days 4.01 6.12 4.49 5.35

(a) Compressive strength of geopolymer brick at different NaOH concentration

and FS
10
Compressive strtength (MPa)

0
SA-3-6 SA-3-8 SA-3-10 SA-3-8
3-days 6.35 6.7 4.86 5.4
7-days 6.4 7.1 5.77 5.44
14-days 6.89 7.6 6.62 6.3
28-days 6.19 7.9 7.33 6.6

(b) Compressive strength of geopolymer brick at different NaOH concentration

and Si/Al =3.4
12

10
Compressive stength (MPa)

0
FS-8 SA-1-8 SA-2-8 SA-3-8 SA-4-8 SA-5-8
3-days 5.2 5.4 5.6 6.7 7.5 6.7
7-days 5.3 5.7 5.9 7.1 8.1 6.5
14-days 5.9 6.09 6.2 7.6 9.5 6.3
28-days 6.1 6.84 7.6 7.9 10.9 5.5

(c) Compressive strength at different Si/Al ratios with 8M NaOH

Fig. 5. Compressive strength of geopolymer brick, (a) Compressive strength of geopolymer brick at different NaOH concentration and FS, (b)
Compressive strength of geopolymer brick at different NaOH concentration and SiAl = 3.4, (c) Compressive strength at different Si/Al ratios with
8 M NaOH.

geopolymer network [69]. These products fill the pores, increasing the density [63].
The products of the polymerization process are divided into two large groups, based on the content of CaO contained in their
chemical composition. The first group: materials with low content of calcium (Ca / (Si + Al) < 1) as low calcium materials, also called
as geopolymers, mostly they are called aluminum silicate. At undergoing to geopolymeric reaction, it forms compounds similar to
zeolite, which are highly crystalline or nano-crystalline. Addition to, it containing an amorphous gel called N-A-S-H, this list included
fly ash and metakaolin. The phases of the alkaline activation reaction of these substances are defined, through the phases of disso­
lution, condensation, reorganization, polycondensation, with or without crystallization, and finally solidification [70]. The second
group: Substances containing large amounts of calcium (Ca / (Si + Al) > 1) of these precursors are blast furnace slag, and their tart is
alkali activated similar to Portland cement, but gels called C-A-S-H (tobermorite) are formed. In addition, some byproducts are formed
in this reaction, as is the case with N-A-S-H and hydrotalcite[70,71].
The high content of alumina (i.e., low Si/Al ratio) in sample SA-5 reduced the compressive strength of the bricks [72,73]. Kouamo
et al. [39] tested the effect of adding different percentages of alumina (10%, 20%, 30%, 40%) as replacements of kaolin on the

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compressive strength, demonstrating that the 20% alumina is considered the optimum percentage as the compressive strength is
increased by 18.1% compared to that of kaolin-geopolymer. A high alumina content will lead to the formation of a less homogeneous
microstructure and cracks because of the non-dissolved particles in the gelatinous matrix of materials, reducing the compressive
strength. A high Al content forms an octahedral Al that cannot be combined with the gel network [74]. Geopolymerization is a
chemical reaction, proceeding and complete with increasing the reaction time [49,75]. In other words, a long curing time enhanced the
degree of geopolymerization, subsequently increasing the strength. Thus, the increase in alumina and curing age were favorable to the
dissolution of alumina and silicate species, consequently enhancing the formation of [SiO (OH)3]- and [Al (OH)4]- intermediates.
Accordingly, polycondensation and the formation of a polymeric binder improved the compressive strength. At Si/Al ratios lower than
the optimal ratio, the strength decreased due to the unbalanced amounts of tetrahedral SiO4 and AlO− 4, and Na+ cations, which led to
the low stability of geopolymer systems [76]. Furthermore, the presence of Al in Al (OH)4 required a sufficient concentration of Na+ to
charge balance the Al (OH)4 group. However, when the Si/Al ratio exceeded the optimal ratio, the strength decreased due to the
formation of highly soluble Si-O- and the low Al and Na2O contents. Consequently, the reaction products did not have enough time to
interact with the alkaline solution, producing unreacted particles. In a proper geopolymer mixture, the reaction products developed
with extended in curing age, which led to the formation of a proper geopolymer network and the subsequent enhancement of the
compressive strength [76]. Fig. 6 shows the effect of the addition of Al on the compressive strength of thermal insulation geopolymer
bricks. Therefore, the inclusion of Al as a partial substitute of 1%, 2%, 3% and 4% of Si mass increased the compressive strength
upward, the rate of increase was 112%, 124%, 129% and 178% at test age 28-day test life, respectively, compared to reference mix. On
the other hand, inclusion of Al as a partial substitute with 5% of Si mass caused the opposite result, compressive strength decreased to
90% compared to the reference mixture at test age 28-day.

3.3. Bulk density

Fig. 7A and B show the effect of NaOH concentration on the bulk density of the FS and SA-3 brick samples. The maximum bulk
density was attained at 8 M NaOH for both samples at different curing ages. The concentration of alkaline solution plays an important
role in the evaluation of the variation of bulk density due to increased geopolymerization and reduced porosity of the body [77]. The
decrease in the Si/Al ratio by the addition of AW to FS increased the bulk density at different curing ages and with 8 M NaOH (Fig. 7C).
The maximum density (1599 kg/m3) was obtained by SA-4-8, which is consistent with the compressive strength. This increase in
density could be due to the increase in alumina, which increased the compactness and reduced the porosity of the brick samples. The
compressive strength and the density decreased with the increasing Si/Al ratio because of the amount of unreacted materials in the
specimens, which act as defect sites [41].

3.4. Water absorption and apparent porosity

The water absorption was determined using the ratio of the mass of water absorbed in the saturated case to the mass of dry
specimen. Fig. 8 shows the effect of adding AW in both the cold and boiling water absorptions of the brick samples, respectively, at 8 M
NaOH and different curing ages. The cold and boiling water absorptions decreased with the increasing alumina. This observation is
consistent with the bulk density results. Furthermore, the decrease in water absorption could be attributed to the decrease in pores
accompanying the AW addition. Alumina enhanced the geopolymerization process and assisted in the incarceration of the unreacted/
partially reacted crystalline phase of the starting material [39]. Furthermore, to compensate for the alumina shortage in FS, part of the
AW can be used as an aggregate to fill some of the pores in the brick samples, consequently reducing the water absorption capacity with
increase in density and compressive strength. The apparent porosity is compatible with the percentage of water absorption (Fig. 9). The
porosity decreased with the increasing AW content (low Si/Al ratio). The large increase in pore volume of the geopolymers was
observed with the increasing Si/Al ratio [41].

Fig. 6. Compressive strength of the samples (S-A-(1, 2, 3, 4 and 5)) compared to the reference sample (FS).

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M.M. Ahmed et al. Case Studies in Construction Materials 15 (2021) e00737

Fig. 7. Bulk density of geopolymer brick, (a) Bulk density at different NaOH concentration with SiAl = 1.15, (b) Bulk density at different NaOH
concentration with SiAl = 4.3, (c) bulk density at different Si/Al with 8 M NaOH.

3.5. Thermal conductivity

The thermal conductivities of the six brick samples were determined at different proportions of AW after 28 curing days and with
8 M NaOH (Fig. 10). Fig. 10 indicates that the thermal conductivity decreased with the increase in AW content. The thermal con­
ductivities of alumina and silica were the lowest among the ceramic materials [78]. Thus, alumina was utilized as a refractory material.
Sample FS-8 exhibited the highest thermal conductivity due to the presence of unreactive silicon in the FS, which is a good conductor.
Sample SA-4-8 exhibited a low thermal conductivity of 0.33 W/m*k, which is lower than those of conventional perforated clay bricks
(~0.8 W/m*k) and even clay bricks with induced porosity (~0.4 W/m*k) [79,80]. Sample SA-5-8 displayed the lowest thermal
conductivity (0.28 W/m*k) and a compressive strength that is lower than the standard. Table 6 presents a comparison of some geo­
polymer foam characteristics based on the literature with those of our prepared geopolymer foam.

3.6. FTIR analysis

Fig. 11 shows the FTIR spectra of FS and the prepared geopolymer bricks (i.e., SA-1-8, SA-3-8, and SA-4-8) after the curing age of 28

9
M.M. Ahmed et al. Case Studies in Construction Materials 15 (2021) e00737

Cold water absorp�on (%)

40

35

30

25

20

15

10

0
FS-8 SA-1-8 SA-2-8 SA-3-8 SA-4-8 SA-5-8
28-days 24.1 23.9 21.1 18.6 15.7 15.8

(a) Cold water absorption of geopolymer brick of different Si/Al mixtures at 8M

NaOH.
Boiling water absorp�on (%)

40

35

30

25

20

15

10

0
FS-8 SA-1-8 SA-2-8 SA-3-8 SA-4-8 SA-5-8
28-days 29.3 28.3 26.2 22.5 18.7 20.3

(b) boiling water absorption

Fig. 8. Water absorption of geopolymer brick of different Si/Al mixtures at 8 M NaOH, (a) Cold water absorption of geopolymer brick of different
Si/Al mixtures at 8 M NaOH, (b) boiling water absorption.

Fig. 9. Apparent porosity of geopolymer bricks of different Si/Al mixtures at 8 M NaOH.

Fig. 10. Thermal conductivity of geopolymer bricks of different Si/Al mixtures at 8 M NaOH.

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M.M. Ahmed et al. Case Studies in Construction Materials 15 (2021) e00737

Table 6
Compared our geopolymer foam characteristics (e.g., raw materials, bulk density, total porosity, compressive strength and thermal conductivity) with
geopolymer foam characteristics reported on the literature.
Raw material Pore Bulk density Total porosity Compressive strength Thermal Reference
creator (g/cm3) (%) (MPa) conductivity
(W/m*k)

Metakaolin H2O2 66–83 0.3–11.6 [81]

0.37–0.74 0.11–0.17
Fly ash Al 0.89–0.93 – 5.5–10.9 0.25–0.39 [82]
Metakaolin, rice husk ash, and volcanic Si – 64–87 – 0.12–0.25 [83]
ash
Metakaolin H2O2 0.6–1.2 42–73 1.2–7.0 0.1–0.4 [84]
Metakaolin Si 0.3–1. – – 0.08–0.12 [85]
Metakaolin Al 0.8–1.1 – 4.4–9.5 0.3–0.65 [86]
Metakaolin Al 0.36–0.59 75–80 – 0.12–0.17 [87]
SA-4-8 Si 0.71–1.5 40–32 3.8–10.9 0.28-0.59 This study

Fig. 11. FTIR spectra of silica slug and prepared geopolymer bricks, (FS-8, SA-1-8, SA-3-8, and SA-4-8).

days. The broad bands observed at 3450 and 1640 cm− 1 corresponds to the O-H stretching and the H-O-H bending vibrations,
respectively [88,89]. These vibration modes are due to the physically adsorbed water on the surface or trapped in the large cavities
[90]. Water is an important factor in the geopolymerization process, helping in the separation and hydrolysis of solid particles to form
dissolved Al3+ and Si4+ cations [91]. Low-intensity absorption bands appeared at 2920 and 2855 cm− 1, indicating organic matter
(aliphatic structures) [92]. The broad and low-intensity absorption band at 1430 cm− 1 is due to the occurrence of sodium carbonate,
which is consistent with the stretching vibration of the O-C-O bond that might have formed due to the atmospheric carbonation of
alkaline media [93,94]. The Si-O stretching band is located in the range of 1000–1200 cm− 1. The band at 1070 cm− 1 is assigned to the
Si–O stretching in the tetrahedrons characterized by the silicon bound to three bridging oxygen units and one nonbridging oxygen;
these structures are considered the building blocks of geopolymers [88]. The bands between 800 and 500 cm− 1 are associated with the
tetrahedral vibrations of the secondary building unit and the fragments of aluminosilicate; the two bands at 782 and 695 cm− 1 could be
attributed to the asymmetric stretching of the Si-O-Al bonds [89,95]. The band at 461 cm− 1 corresponds to the bending vibration of the
Si-O-Si group [96].

Fig. 12. SEM images of SA-4-8.

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M.M. Ahmed et al. Case Studies in Construction Materials 15 (2021) e00737

3.7. Microstructure

Fig. 12 shows the SEM images of SA-4-8, as can see in the Fig. 12A, the homogeneity in microstructure of geopolymer is clear from
microstructure analysis, as dense and homogenous matrix is formed (Fig. 12B). This observation approves that the suitable Al2O3
addition is preferable to enhance the geopolymerization extent and justifies the compressive strength of samples. These results
confirmed the FTIR results. Furthermore, it can be seen the presence of air bubbles trapped inside the geopolymer. Adjust the trapped
air bubbles contribute by adjust precursors mixture is contributes to obtaining the appropriate mass, mechanical strength, and thermal
characteristics of the geopolymer brick.

4. Conclusion

In the current study, the following points can be drawn:

1. FS can be utilized to produce thermal insulation geopolymer bricks (lightweight bricks) with a compressive strength of 6.1 MPa, a
bulk density of 860.7 kg/m3, an apparent porosity of 40.2%, and a thermal conductivity of 0.59 W/m.k.
2. Alumina can be added to FS to compensate for its alumina deficiency.
3. The results indicate that adding alumina enhanced the geopolymer brick properties of FS at SA-4-8 ratio (particularly the
compressive strength, i.e.,10.9 MPa) after 28 days. However, the addition of aluminum at SA-5-8 ratio decreased the compressive
strength of the prepared geopolymer brick to 5.5 MPa after 28 days.
4. The geopolymer brick sample with a SiO2/Al2O3 ratio = 1 achieved a higher compressive strength (10.9) than the other SiO2/
Al2O3 ratios (4, 3, 2, 0.5) and the pristine FS after 28 days of curing and at 8 M NaOH.
5. The increase in AW decreased the thermal conductivity, water absorption, and apparent porosity of the prepared geopolymer brick
to 0.28 W/m.k, 20%, and 33.09% for the SA-5-8 sample, respectively. Meanwhile, the compressive strength and the bulk density
were 5.5 MPa and 1680.2 kg/m3, respectively.

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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