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The Effect of Finely-Grinded Crushed Brick Powder on Physical and

Microstructural Characteristics of Lightweight Concrete

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DOI: 10.3390/min12020159

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 minerals
Article
The Effect of Finely-Grinded Crushed Brick Powder on Physical
and Microstructural Characteristics of Lightweight Concrete
Hussein Al-kroom 1, * , May M. Atyia 2, * , Mohamed G. Mahdy 2 and Mohamed Abd Elrahman 2






Citation: Al-kroom, H.; Atyia, M.M.;
Mahdy, M.G.; Abd Elrahman, M. The
Effect of Finely-Grinded Crushed
Brick Powder on Physical and
Microstructural Characteristics of
Lightweight Concrete. Minerals 2022,
12, 159. https://doi.org/10.3390/
min12020159
Academic Editor: Dawei Wang
Received: 25 December 2021
Accepted: 26 January 2022
Published: 27 January 2022
Publisher’s Note: MDPI stays neutral
with regard to jurisdictional claims in
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iations.
Copyright: © 2022 by the authors.
Licensee MDPI, Basel, Switzerland.
This article is an open access article
distributed under the terms and
conditions of the Creative Commons
Attribution (CC BY) license (https://
creativecommons.org/licenses/by/
4.0/).
Minerals 2022, 12, 159. https://doi.org/10.3390/min12020159
1 Civil Engineering Department, The University of Jordan, Amman 11942, Jordan
2 Structural Engineering Department, Faculty of Engineering, Mansoura University, Mansoura 35516, Egypt;
mmahdy@mans.edu.eg (M.G.M.); mohamedattia@mans.edu.eg (M.A.E.)
* Correspondence: h.alkroom@ju.edu.jo (H.A.-k); may.atyia92@gmail.com (M.M.A.)
Abstract: The utilization of waste crushed clay brick (CB) in concrete reduces its harmful impacts
on the environment as it can be found in many places around the world. This research studies the
possibility of using clay brick powder (CBP) as a filler material to produce lightweight concrete as
it has been exposed to high temperatures during manufacturing of the bricks, which increases its
pozzolanic reactivity. The effect of using an air-entraining agent (AEA) for additional pore formation
on concrete performance was evaluated. Eight mixtures were prepared and examined to achieve the
research objectives. Concrete flowability, dry density, compressive strength, ultrasonic pulse velocity,
thermal conductivity, sorptivity, and porosity were measured. Additionally, scanning electron
microscopy, X-ray diffraction, thermo-gravimetric analysis, and mercury intrusion porosimetry were
used to analyze the microstructure characteristics of the concrete. The results indicate that the use
of CBP as filler material enhances the mechanical and durability characteristics of the concrete. In
contrast, adding an AEA has negative effects on concrete’s mechanical and durability properties, but
on the other hand, its use enhances the thermal properties of the concrete.
Keywords: porosity; air-entraining agent; crushed clay brick concrete; microstructure
1. Introduction
Construction and demolition wastes represent serious environmental problems as they
occupy rare landfills. These wastes cause damage to the land as they dissolve, producing
harmful substances which pollute the soil and water [1,2]. One of these wastes is crushed
clay brick (CB) waste. Brick is also considered a waste material when it breaks during
the production process or when it does not meet standards. CB waste is transported to
landfills or dumped into designated sites [3,4]. This waste is increasing annually, which
increases the need for huge waste landfills [5]. Due to the limited number of landfills,
CB waste occupies valuable landfills and damages soil structure, resulting in poor grain
yield. Waste storage has become a serious environmental problem. Therefore, CB waste
should be reused to significantly reduce the waste that will be transported to landfills [6].
CB’s first use in concrete was in 1860. After that, it was used as aggregate in concrete for
the first time after World War II [7]. CB waste is usable in building materials based on
concrete as an artificial recycled aggregate [8]. Aggregates represent about (60%−75%)
of concrete volume. Therefore, if CB waste were to be recycled as aggregates in concrete
production, this would preserve significant natural aggregate resources and consume large
quantities of CB wastes [9]. The influence of utilizing CB as coarse aggregate in concrete
has been investigated in several studies [9–13]. The incorporation of CB as fine aggregate
in the concrete industry has been evaluated [14–18]. The utilization of CB as coarse and
fine aggregates in concrete production has been investigated [1,2]. Using CB as aggregate
decreases the concrete workability [14]. The compressive strength of concrete made with
CB as aggregate is weaker than that of the concrete produced with normal aggregates [10].
However, utilizing it as aggregate in concrete reduces the concrete weight [1].
https://www.mdpi.com/journal/minerals
Minerals 2022, 12, 159 2 of 17

Lightweight concrete has been widely used in construction for many years. Its use is
preferred because of its low density and good sound and thermal insulation [10,19]. Using
this type of concrete decreases the structure’s dead weight, which causes a reduction in
the construction cost as its use reduces the foundation size and also reduces the size of the
structural elements [20]. Lightweight concrete has a wide range of densities, which makes
its application field wider. It can be classified into two types: cellular concrete produced
by creating air voids in the concrete and lightweight aggregate concrete produced using
lightweight aggregate from natural sources or manufactured with raw materials [21,22].
CB aggregates can be used to produce lightweight aggregate concrete. Its use would
not only reduce CB waste but also produce lightweight aggregate concrete with more
environmentally, friendly, and cheaper materials [2]. The production of lightweight concrete
using CB as an aggregate has been investigated as shown in Table 1.

Table 1. Summary of research that examined the production of lightweight concrete with CB.

References Production Compressive Strength (Mpa) Dry Density (kg/m3 )

Zhao et al., 2018 [2] Lightweight aggregate concrete 32.6–40.2 1729–1850
Structural lightweight
Atyia et al., 2021 [4] ≥27 ≤1860
aggregate concrete
Wongsa et al., 2018 [22] Lightweight geopolymer concrete 8.2–18.3 1685–1749
Structural lightweight
Noaman et al., 2021 [23] 27.2–27.8 1926–1960
aggregate concrete

In the process of air entrainment, small air bubbles are generated in the concrete.
These air bubbles become part of the cement matrix [24]. Three methods can be used
to achieve these air bubbles and produce air-entraining concrete. The first method is
achieved by adding an air-entraining agent (AEA) with other concrete components during
the mixing process. The second one is achieved by using air-entraining cement, which
includes an air-entraining agent as an addition interground with the clinker during the
manufacturing process of the cement. The third method is a combination of the first method
and second method. AEA addition can improve the resistance to freezing and thawing as
it produces dispersed and distributed air bubbles [25]. The effect of adding an AEA with
different dosages on the characteristics of the concrete was studied [20,26–29]. Deng et al.
used Rosin acid sodium with a dosage of 0.05% of cement weight as an AEA. Adding an
AEA causes an increase in the ratio of mesopores and macropores, which causes a decrease
in the dry density [26]. With increasing the AEA content, the proportion of the pores with a
diameter more than 0.3 mm increases [27]. The concrete compressive strength decreases
with increasing the percentage of AEA [27–29]. The utilization of the AEA lowers the
tensile strength [29]. The utilization of the AEA improves the frost resistance of the concrete
as it increases the porosity of the concrete [26]. Increasing the AEA causes an increase in the
water penetration depth [25]. Increasing the AEA content increases the water absorption of
concrete [28,29]. The application of the AEA increases the air permeability and the moisture
content [29]. The influence of utilizing the AEA in producing the mortar was studied. The
compressive strength and the unit weight decreased with increasing the AEA content [30].
Most studies have investigated the effect of utilizing CB as fine aggregate in producing
cement-based materials or coarse aggregate in producing concrete. A few investigations
have studied the properties of concrete containing CB as fine and coarse aggregates. Only a
few studies have studied the effect of utilizing clay brick powder (CBP) as filler material in
producing cement-based materials. A few studies investigated the effect of adding an AEA
in cement-based materials.
The main objectives of this research were to determine the effect of using CBP as a
filler material and the influence of adding the AEA in crushed clay brick concrete. The
fresh and hardened properties of the CB aggregate concrete were studied in this research.
The absorption of the obtained concrete was determined to measure the durability-related
characteristics. The thermal conductivity of the concrete was evaluated to determine the
 material in producing cement-based materials. A few studies investigated the effect of
adding an AEA in cement-based materials.
The main objectives of this research were to determine the effect of using CBP as a
filler material and the influence of adding the AEA in crushed clay brick concrete. The
Minerals 2022, 12, 159 fresh and hardened properties of the CB aggregate concrete were studied in this research. 3 of 17
The absorption of the obtained concrete was determined to measure the durability-related
characteristics. The thermal conductivity of the concrete was evaluated to determine the
insulation
insulation properties
properties of
of the
the obtained
obtained concrete.
concrete. Scanning
Scanning electron
electron microscopy
microscopy (SEM),
(SEM), X-ray
X-ray
diffraction (XRD), thermo-gravimetric analysis (TGA), and mercury intrusion porosime-
diffraction (XRD), thermo-gravimetric analysis (TGA), and mercury intrusion porosimetry
try
(MIP)(MIP)
werewere
usedused to analyze
to analyze the the microstructural
microstructural properties
properties of obtained
of the the obtained concrete.
concrete.

2. Materials
Materials
CB from construction wastes was utilized utilized inin this
this investigation.
investigation. ItIt was manually
crushed and graded into sizes to be used as coarse aggregate and fine aggregate. Coarse
crushed clay brick aggregate (CCB) with a maximum nominal size of 12.5 mm was utilized
as coarse aggregate. Fine crushed clay brick aggregate (FCB) with 2.74 fineness modulus
was used as fine aggregate. Aggregates were tested according to EN ISO 19595 [31]. Clay
brick powder (CBP) with particle size less than 0.125 mm was used as filler material. material. It
was used as a replacement material for fine aggregate. Figure Figure 1 shows the crushed clay
brick aggregate (CCB, FCB, and CBP). Ordinary Portland cement CEM I 52.5 N meets the
requirements of ES 4756-1 [32]. Silica
requirements Silica fume
fume (SF)
(SF) complying
complying withwith ASTM
ASTM C C 1240
1240 [33] was
used as a partial replacement for cement. Oxide Oxide compositions
compositions of of cement,
cement, SF,
SF, and CBP are
Figure 22 presents
illustrated in Table 2. Figure presents the
the particle
particle size
size distributions
distributions of
of the
theused
usedmaterials.
materials.
Superplasticizer (SP),
Superplasticizer (SP), which
which confirms
confirms thethe requirements
requirements of of ASTM
ASTM C C 494
494 type F [34], was
utilized as
utilized as aa high
high water
waterreducer.
reducer.Aqueous
Aqueoussynthetic
syntheticresin-type
resin-typedispersions
dispersions asas
air-entraining
air-entrain-
concrete admixture was used as an AEA. It complies with ASTM
ing concrete admixture was used as an AEA. It complies with ASTM C 260-81 C 260-81 [35]. Its [35]. Its
density
is 1.01 kg/L. It was used to produce lighter concrete.
density is 1.01 kg/L. It was used to produce lighter concrete.

(a) (b) (c)

Figure
Figure 1.
1. Crushed
Crushed clay
clay brick
brick aggregate:
aggregate: (a)
(a) CCB
CCB (b),
(b), FCB,
FCB, and
and (c)
(c) CBP.
CBP.

Table 2. Oxide compositions of the used materials.

Table 2. Oxide compositions of the used materials.
Oxide Composition (%) Cement SF CBP
Oxide Composition
SiO2 Cement 20.15 SF 90.18 CBP51.6
(%)
Fe2O3 3.25 0.35 10.40
SiO2 20.15 90.18 51.6
Fe2 O3 Al2O3 3.25 6.1 0.35 0.47 10.4014.0
Al2 O3 CaO 6.1 62.6 0.47 0.56 14.07.15
CaO MgO 62.6 1.9 0.56 4.32 7.151.67
MgO SO3 1.9 2.4 4.32 0.26 1.677.66
SO3 2.4 0.26 7.66
TiO2
TiO 2
0.3
0.3 0.22
0.22 1.82
1.82
Loss on Ignition
Loss on Ignition 1.7 1.7 2.9 2.9 1.741.74
Minerals 2022, 12, 159 4 of 17
Minerals 2022, 12, 159 4 of 17

100
90
80 CCB

70
Under size (%) FCB
60
50 CBP
40
Cement
30
20 SF
10
0
0.01 0.1 1 10 100 1000 10000
Diameter (µm)

Figure
Figure 2. Particle
2. Particle sizesize distributions
distributions of coarse
of coarse crushed
crushed clayclay brick
brick aggregate
aggregate (CCB),
(CCB), finefine crushed
crushed clay
clay
brick aggregate
brick aggregate(FCB),
(FCB),clay brick
clay powder
brick powder(CBP), cement,
(CBP), and
cement, silica
and fume
silica (SF).
fume (SF).

3. Mix Proportioning
3. Mix Proportioning
ToToachieve
achieve thethe
objective
objective of the research,
of the research,eight mixtures
eight mixtures were designed
were designed andandprepared.
prepared.
Table 3 presents the proportions of the concrete mixtures that
Table 3 presents the proportions of the concrete mixtures that were designed using were designed using thethe
absolute volume method. CBP was used as fine aggregate with different
absolute volume method. CBP was used as fine aggregate with different ratios (0 wt.%, ratios (0 wt.%, 10
wt.%, 20 wt.%, and 30wt.%) in (MF0, MF10, MF20, and MF30),
10 wt.%, 20 wt.%, and 30wt.%) in (MF0, MF10, MF20, and MF30), respectively. In other respectively. In other
mixes,
mixes,an an
AEA AEA was used
was used with
with(0.25%, 0.5%,
(0.25%, 0.75%,
0.5%, 0.75%,andand1%) weight
1%) weightratios in in
ratios cementitious
cementitious
materials
materials in mixes
in mixes(MF30-0.25,
(MF30-0.25, MF30-0.
MF30-0.5, MF30-0.75, and MF30-1),
5, MF30-0.75, and MF30-1),respectively. All ag-All
respectively.
gregates werewere
aggregates usedused
in saturated
in saturatedand and
surface dry dry
surface (SSD) conditions
(SSD) conditionsbefore
beforemixing.
mixing.A mixer
A mixer
with
witha capacity
a capacity of of
0.07 m3m
0.07 3 was
was utilized to mix
utilized thethe
to mix components
components of the mixtures.
of the mixtures. Coarse
Coarseandand
fine aggregates were mixed in the mixer for 2 min, and then cementitious
fine aggregates were mixed in the mixer for 2 min, and then cementitious materials were materials were
added
added and mixed
and mixedforfor
2 min.
2 min.A total
A totalof of
2/32/3
of the water
of the waswas
water added
added andandmixed
mixed for for
2 min.
2 min.
Then
Then1/31/3
of the water
of the mixed
water mixedwith SP SP
with waswasadded
addedandand
mixed
mixedforfor
2 min.
2 min.In mixes
In mixes containing
containing
an an AEA,
AEA, it was
it was added
added to to
thethe mixer
mixer andand mixed
mixed forfor only
only anan extra
extra 2 min.
2 min. TheThe flowability
flowability of of
thethe obtained
obtained concrete
concrete was was immediately
immediately measured,
measured, andand then
then thethe fresh
fresh concrete
concrete was was cast
cast in in
steel
steel molds.
molds. TheThe samples
samples were
were demolded
demolded after
after 24 24 h and
h and then
then cured
cured in water.
in water. The The samples
samples
were then taken out of the water at the testing date, and the
were then taken out of the water at the testing date, and the hardened properties were hardened properties were
measured.
measured. SEM,SEM,XRD,XRD,TGA,TGA, and and
MIPMIP were
were also
also analyzed.
analyzed.

Table
Table 3. Mixture
3. Mixture proportions
proportions of of
thethe concrete
concrete 3). 3 ).
(kg/m
(kg/m

Components
Components (kg/m3) (kg/m3)
Mix Label Mix Label
CCB FCB CCB
CBP FCB
Cement CBP SF Cement SF
water water
SP SP AEA
AEA
MF0 700 700 ‫ـ‬ 432 48 168 7.2 ‫ـ‬
MF0 700 700  432 48 168 7.2 
MF10 700 630 70 432 48 168 7.2 -
MF10 700 630 70 432 48 168 7.2 -
MF20 700 MF20
560 700
140 560
432 140 48 432 16848 1687.2 7.2 ‫ـ‬
MF30 700 490 210 48 432 48 1687.2 7.2 ‫ـ‬
MF30 700 490 210 432 168 
MF30-0.25 700 490 210 432 48 168 7.2 1.2
MF30-0.25 700 490 210 432 48 168 7.2 1.2
MF30-0.5 700 MF30-0.5
490 700
210 490
432 210 48 432 16848 1687.2 7.2 2.4
2.4
MF30-0.75 700 MF30-0.75
490 700
210 490
432 210 48 432 16848 1687.2 7.2 3.6
3.6
MF30-1 700 490
MF30-1 210
700 432
490 210 48 432 16848 1687.2 7.2 4.8
4.8
Minerals 2022, 12, 159 5 of 17

4. Experimental Work
The influence of utilizing CBP as filler material was studied in this investigation.
Additionally, the AEA’s influence was also studied. The fresh and hardened characteristics
of the concrete were evaluated. The flowability was measured by using the slump flow test
according to EN 12350-8 [36]. It was measured using a steel cone with a 30 cm height, 20 cm
lower diameter, and 10 cm upper diameter. It was placed with the bigger opening at the
bottom on a smooth surface. It was filled with fresh concrete, and the surface was leveled.
Then, the cone was slowly raised, and fresh concrete would flow. Two perpendicular
diameters of the concrete were measured to obtain the mean flow diameter value. The test
was performed three times to obtain the average flow diameter value.
To evaluate the hardened characteristics of the concrete, the following tests were used.
The dry density of the concrete was evaluated as per EN 12390-7 [37]. Three 28-day-old
specimens (100 mm cubes) were utilized to evaluate the dry density. The dry mass of each
specimen was determined after drying at 105 ± 5 ◦ C until reaching a constant mass. The dry
density was then calculated by dividing the dry mass by the measured volume. The average
value of the three specimens was used to determine the dry density. The compressive
strength of the concrete was evaluated following BS EN 12390 [38] at 7, 28, and 91 days.
Three 100 mm cube specimens of each age were used to determine the average compressive
strength. A hydraulic testing machine with a capacity of 100 tons and an accuracy of 0.2 ton
was used to test the samples. The direct transmission method was utilized to evaluate the
ultrasonic pulse velocity (UPV) as specified in ASTM C597-16 [39]. Three dried specimens
with dimensions of 100 × 100 × 100 mm3 of each mixture after 28 days were used to
obtain the average value of the UPV. It was calculated by using the computed time and the
concrete length. The concrete sorptivity was measured using three 100 mm cubes at 28 days.
It was evaluated following EN ISO 15148 [40]. Thermal conductivity was measured to
ascertain the thermal insulation capacity of the concrete. It represents the heat loss passing
through dried concrete strips with dimensions of 100 × 100 × 30 mm3 . An electric heater
was utilized as a heat source. A heat recorder and thermocouples were used to measure the
temperature. Fourier’s equation was used to calculate the thermal conductivity coefficient.
Concrete cylinders with a diameter of 25 mm and height of 65 mm taken from the core of
the hardened cube were utilized to evaluate the concrete porosity. The samples were dried
to constant mass, and then the dry density of the sample was measured, and the samples
were placed in the helium pycnometer to measure the specific density of the concrete.
The average specific density was be calculated from the three measured specific densities.
Equation (1) was utilized to obtain the porosity of the hardened concrete at 91 days.

ρs − ρd
∅ H.P = × 100 (1)
ρs

where:
∅ H.P : Total porosity of the concrete (%),
ρs : Specific density (gm/cm3 ),
ρd : Dry density (gm/cm3 ).
For microstructural investigations, SEM, XRD, TGA, and MIP were measured as
follows. SEM was utilized to analyze the influence of utilizing CBP as filler material and
the effect of using different dosages of the AEA. The microstructure investigations of
MF0, MF30, MF30-0.5, and MF30-1 were analyzed by SEM at 91 days. A JEOL JSM-6510LV
scanning electron microscope was used to study the microstructure of the concrete (Electron
Microscopy Unit, Mansoura University, Egypt). An XRD test was performed to ascertain
the concrete microstructure of the selected samples (MF0, MF30, MF30-0.5, and MF30-1)
after 91 days. Dry concrete cubes with dimensions of (100 × 100 × 100 mm3 ) were ground
into powders and analyzed using an X-ray diffractometer. Samples were scanned with
a speed of 2◦ /min over an interval from 5◦ to 50◦ . An X’PertHighScore 2006 program
with the ICDD (International Center for Deviation Data) database was used to measure
Minerals 2022, 12, 159 6 of 17

Minerals 2022, 12, 159 the ICDD (International Center for Deviation Data) database was used to measure6 of the
17
most probable phases (HBRC, Cairo, Egypt). For more microstructure investigations, sam-
ples (MF0, MF30, MF30-0.5, and MF30-1) were analyzed by TGA. Concrete cubes at 91
days were ground into powders. Samples were heated at a rate of 20 °C/min up to 1000
the most probable phases (HBRC, Cairo, Egypt). For more microstructure investigations,
°C under(MF0,
samples a dynamic
MF30,nitrogen
MF30-0.5, atmosphere
and MF30-1) by awere
TGA-50 thermal
analyzed by analyzer
TGA. Concrete(HBRC,cubesCairo,at
Egypt). MIP was utilized to assess the pore structure of the
91 days were ground into powders. Samples were heated at a rate of 20 C/min up concrete at 91 days.
◦ The sam-to
ples
1000were smallapieces
◦ C under dynamic withnitrogen
diameters between 2by
atmosphere mm and 4 mm
a TGA-50 taken analyzer
thermal from the (HBRC,
central
part of hardened concrete. Before the test, samples of MF0, MF30,
Cairo, Egypt). MIP was utilized to assess the pore structure of the concrete at 91 days. MF30-0.5, and MF30-1
were dried. Then,
The samples werethe dried
small samples
pieces withwere loadedbetween
diameters in the testing
2 mmchamber
and 4 mm of taken
an MIP device
from the
(Micromeritics pore sized 9320, automatic mercury intrusion pore
central part of hardened concrete. Before the test, samples of MF0, MF30, MF30-0.5, and size analyzer). The
pressure
MF30-1 werewas dried.
vacuumed Then,from the testing
the dried samples chamber, then in
were loaded thethe
mercury
testing intrusion
chamber of pressure
an MIP
was performed progressively from 1 psi (8.6 kPa) to a maximum
device (Micromeritics pore sized 9320, automatic mercury intrusion pore size analyzer). pressure of 30,000 psi
(206.84 MPa). The pore size of the specimens, which was within
The pressure was vacuumed from the testing chamber, then the mercury intrusion pressure the range from 6 nm to
about 170 µm, was detected and recorded. The equilibrium time
was performed progressively from 1 psi (8.6 kPa) to a maximum pressure of 30,000 psi for each applied pressure
step wasMPa).
(206.84 set asThe
10 s.pore
The size
contact angle
of the betweenwhich
specimens, the mercury
was withinand thethepores
rangewas from130°.
6 nm Theto
surface
about 170tension of the
µm, was mercury
detected was
and 485 dynes/cm,
recorded. and its density
The equilibrium time was 13.53applied
for each g/mL (CMRDI,
pressure
Cairo,
step was set as 10 s. The contact angle between the mercury and the pores was 130◦ . The
Egypt).
surface tension of the mercury was 485 dynes/cm, and its density was 13.53 g/mL (CMRDI,
5. Results
Cairo, and Discussion
Egypt).
5.1. Fresh Properties (Flowability)
5. Results and Discussion
The slump flow test was used to evaluate the performance of the fresh concrete. The
5.1. Fresh Properties (Flowability)
results of the slump flow test for the fresh concrete are illustrated in Figure 3. The values
were The
foundslump
to beflow test was
between 500used
andto 700evaluate the performance
mm without of the fresh
any segregation. concrete.
The figure The
shows
results of the slump flow test for the fresh concrete are illustrated in
that using CBP as filler material increased the flowability of the fresh concrete. There was Figure 3. The values
awere found
17.6% to beinbetween
increase 500 andof700
the flowability mmcompared
MF30 without any withsegregation.
MF0. This may The befigure
due shows
to the
increased powder content in the fresh concrete. It was also found that the AEAThere
that using CBP as filler material increased the flowability of the fresh concrete. was
addition
a 17.6% increase in the flowability of MF30 compared with MF0. This
enhanced the flowability as it improved the workability of the fresh concrete. This is sim- may be due to the
increased powder content in the fresh concrete. It was also found that the AEA addition
ilar to the findings found in previous research (Kim et al., 2012 [22] and Tarhan et al., 2021
enhanced the flowability as it improved the workability of the fresh concrete. This is similar
[31]).
to the findings found in previous research (Kim et al., 2012 [22] and Tarhan et al., 2021 [31]).

800

700

600
Slump flow (mm)

500

400

300

200

100

0
MF0 MF10 MF20 MF30 MF30-0.25 MF30-0.5 MF30-0.75 MF30-1

Figure 3.
Figure Slump flow.
3. Slump flow.

5.2. Hardened Properties

5.2.1. Dry Density
Concrete dry density is an important characteristic that has to be studied in SLWAC.
According to DIN 1045-1 [41], SLWAC is concrete that has a dry density of less than
2000 kg/m3 at 28 days. Figure 4 shows the concrete dry density at 28 days. In mixtures
containing CBP as filler material, it was observed that increasing the CBP content increased
the dry density from 1850 kg/m3 in MF0 to 1870 kg/m3 in MF30. This is because CBP
 5.2.1. Dry Density
Concrete dry density is an important characteristic that has to be studied in SLWAC.
According to DIN 1045-1 [41], SLWAC is concrete that has a dry density of less than 2000
kg/m3 at 28 days. Figure 4 shows the concrete dry density at 28 days. In mixtures contain-
Minerals 2022, 12, 159 7 of 17
ing CBP as filler material, it was observed that increasing the CBP content increased the
dry density from 1850 kg/m3 in MF0 to 1870 kg/m3 in MF30. This is because CBP use filled
the voids, and therefore, it caused an increase in the dry density. This is in good agreement
use filled
with theetvoids,
Mobili and
al. [19], therefore,
who found an it caused
increaseaninincrease in thedensity
the concrete dry density.
when This
CBP is
wasin used
good
agreement
as with Mobili
filler material. et al.containing
In mixtures [19], who AEA,
foundits anaddition
increasewas
in the concrete
observed density
to cause when
a signif-
CBP was
icant used as
decrease in filler material.
the dry In It
density. mixtures containing
decreases AEA, its the
with increasing addition
AEA was observed
dosage. This tois
cause a significant decrease in the dry density. It decreases with increasing
because it creates air voids, which increase with increasing the amount of AEA in the the AEA dosage.
con-
This iscausing
crete, because it creates
a lower dryair voids,These
density. whichfindings
increasearewith increasing the
in agreement withamount of AEA
previous studiesin
the concrete, causing a lower dry density. These findings are in agreement
(Deng et al., 2021 [27] and Abd Elrahman et al., 2020 [23]). The lowest dry density was with previous
studies
1746 (Deng
kg/m et al., 2021 [27] and Abd Elrahman et al., 2020 [23]). The lowest dry density
3 in MF30-1.
was 1746 kg/m3 in MF30-1.

1900

1850
Dry density(kg/m3)

1800

1750

1700

1650

1600
MF0 MF10 MF20 MF30 MF30-0.25 MF30-0.5 MF30-0.75 MF30-1

Figure 4.
Figure Concrete dry
4. Concrete dry density.
density.

5.2.2. Compressive Strength

5.2.2. Compressive Strength
The mechanical properties of the hardened concrete were evaluated by measuring
The mechanical properties of the hardened concrete were evaluated by measuring
the compressive strength of the concrete. The values of the compressive strength of the
the compressive strength of the concrete. The values of the compressive strength of the
hardened concrete at 7, 28, and 91 days are plotted in Figure 5. The figure indicates that
hardened concrete at 7, 28, and 91 days are plotted in Figure 5. The figure indicates that
CBP use as filler material enhances the compressive strength at all ages. These results
CBP use as filler material enhances the compressive strength at all ages. These results con-
concur with the findings of a previously reported study (Mobili et al., 2018 [19]). The
cur with the findings of a previously reported study (Mobili et al., 2018 [19]). The com-
compressive strength increased as the CBP content increased. When using CBP as filler
pressive strength increased as the CBP content increased. When using CBP as filler mate-
material, the pores were significantly reduced, and the concrete compressive strength
rial, the pores were significantly reduced, and the concrete compressive strength in-
increased. The increase in the concrete compressive strength increased with time. This
creased. The increase in the concrete compressive strength increased with time. This may
may be because of the pozzolanic activity of the fine particles of the clay brick, which
be because
reacts withofcalcium
the pozzolanic
hydroxide,activity of the fine
producing particles
calcium of the
silicate clay brick,
hydrate which
that fills the reacts
pores
with calcium hydroxide,
and increases producing
the compressive calcium
strength silicate
at later ages.hydrate that fills the
The compressive pores reached
strength and in-
creases
41 MPathe compressive
at 91 days in MF30.strength at later
The AEA ages. The
addition compressive
decreased strength reached
the compressive strength.41 MPa
This
at 91 days in MF30. The AEA addition decreased the compressive strength. This
is because it creates air-entrained voids in the cement matrix, which makes the concrete is because
itweaker.
createsThe
air-entrained
volume ofvoids
thesein the cement
voids matrix,
is related to thewhich
contentmakes theAEA.
of the concrete weaker. The
The compressive
volume
strengthofdecreased
these voids is related
with to the
increasing thecontent of the AEA.
AEA content, Theiscompressive
and this strength
consistent with de-
previous
creased with increasing the AEA content, and this is consistent with previous
studies (Chung et al., 2014 [28] and Tarhan et al., 2021 [31]). This decrease is because the studies
air entrained voids would collapse and produce bigger voids when increasing the AEA
dosage. The compressive strength decreased from 41 MPa in MF30 to 34 MPa in MF30-1.
All studied mixtures were considered SLWAC because all mixtures had a compressive
strength of more than 20 MPa and a dry density of lower than 2000 Kg/m3 , which meet the
requirements of DIN 1045-1 [41].
 trained et
(Chung voids would
al., 2014 collapse
[28] and produce
and Tarhan bigger
et al., 2021 voids
[31]) when
. This increasing
decrease the AEA
is because the dosage.
air en-
The compressive strength decreased from 41 MPa in MF30 to 34 MPa in MF30-1.
trained voids would collapse and produce bigger voids when increasing the AEA dosage.
All studied strength
The compressive mixturesdecreased
were considered
from 41SLWAC because
MPa in MF30 to all mixtures
34 MPa had a compres-
in MF30-1.
siveAll
strength of more than 20 MPa and a dry density of lower
studied mixtures were considered SLWAC because all mixtures had than 2000 Kg/m 3, which
a compres-
Minerals 2022, 12, 159 meetstrength
sive the requirements
of more thanof DIN 1045-1
20 MPa and[41].
a dry density of lower than 2000 Kg/m3, which 8 of 17
meet the requirements of DIN 1045-1 [41].
7 Days
45 728 Days
Days
91 Days
28 Days
45
40
91 Days

(MPa)
40
35

(MPa)
35
strength
30
strength
Compressive 30
25
25
20
Compressive

20
15
15
10
105

50

0 MF0 MF10 MF20 MF30 MF30-0.25 MF30-0.5 MF30-0.75 MF30-1

MF0 MF10 MF20 MF30 MF30-0.25 MF30-0.5 MF30-0.75 MF30-1
Figure 5. Concrete compressive strength.
Figure 5. Concrete compressive strength.
Figure 5. Concrete compressive strength.
5.2.3. Ultrasonic
5.2.3. Ultrasonic Pulse
Pulse Velocity
Velocity
The
5.2.3. The ultrasonic
Ultrasonic pulse
Pulse
ultrasonic velocity (UPV)
Velocity
pulse velocity (UPV) values
values ofof the
the concrete
concreteafter
after 28
28 days
days are
are indicated
indicated
in Figure 6. From
The ultrasonic
in Figure 6. From thethe figure,
pulse velocity
figure, it is clear
(UPV)
it is clear that the
values
that UPV value
of thevalue
the UPV increased
concrete when
after 28when
increased daysthethe content
arecontent
indicated of
of
inthe filler
theFigure material,
6. From the
filler material, CBP, was
figure,
CBP, increased. This
it is clear that
was increased. is
This the because
UPV value
is because using
using CBP
increasedas filler
when
CBP as filler material fills
the content
material the
of
fills the
voids,
voids,
the fillerwhich
which increases
increases
material, the
CBP,the solid
wassolid partand
part
increased. and decreases
decreases
This theusing
the
is because voidpart.
void part. AEA
CBP AEA
as usage
usage
filler reduces
reduces
material UPV
fillsUPV
the
valueswhich
values
voids, dueto
due toincreases
thevoids
the voids that
that
the have
have
solid been
been
part generated
andgenerated
decreasesas as
theaaresult
resultpart.
void ofadding
of adding it. The
it.
AEA usage The UPV values
UPV
reduces values
UPV
increase
increase with
with using
using CBP
CBP as
as filler
filler material
material and
and decreased
decreased with
with adding
adding
values due to the voids that have been generated as a result of adding it. The UPV values AEA.
AEA.
increase with using CBP as filler material and decreased with adding AEA.
3400
3400
3350
(m/s)(m/s)

3350
velocity

3300
velocity

3300
3250
pulse

3250
pulse
Ultrasonic

3200
Ultrasonic

3200
3150
3150
3100
5 3100 MF0 MF10 MF20 MF30 MF30-0.25 MF30-0.5 MF30-0.75 MF30-1
MF0 pulse
Figure 6. Ultrasonic MF10
velocity. MF20 MF30 MF30-0.25 MF30-0.5 MF30-0.75 MF30-1
Figure 6. Ultrasonic pulse velocity.
5.2.4. Thermal Conductivity Coefficient
Figure 6. Ultrasonic pulse velocity.
The thermal conductivity coefficient of the concrete is related to its density and porosity.
The thermal conductivity coefficient values after 28 days are indicated in Figure 7. Using
CBP as filler material in crushed clay brick concrete increased its thermal conductivity. The
thermal conductivity coefficient value of MF30 was higher than that of MF0. This is because
CBP fills the voids, which increases the thermal conductivity coefficient value as the heat
transfers faster in the solid part. It can be seen that using an AEA in concrete reduces its
 5.2.4. Thermal Conductivity Coefficient
The thermal conductivity coefficient of the concrete is related to its density and po-
rosity. The thermal conductivity coefficient values after 28 days are indicated in Figure 7.
Using CBP as filler material in crushed clay brick concrete increased its thermal conduc-
tivity. The thermal conductivity coefficient value of MF30 was higher than that of MF0.
Minerals 2022, 12, 159 9 of 17
This is because CBP fills the voids, which increases the thermal conductivity coefficient
value as the heat transfers faster in the solid part. It can be seen that using an AEA in
concrete reduces its thermal conductivity. This is likely due to the air-entrained voids that
thermal
have beenconductivity. This
created in the is likelybecause
concrete due to the
the air-entrained
AEA was added.voids that have been created in
the concrete because the AEA was added.

0.70

Thermal conductivity coefficient (W/m.K) 0.68

0.66

0.64

0.62

0.60

0.58
MF0 MF10 MF20 MF30 MF30-0.25 MF30-0.5 MF30-0.75 MF30-1

Figure 7. Thermal conductivity coefficient.

Figure 7. Thermal conductivity coefficient.
5.2.5. Sorptivity
5.2.5. Sorptivity
Sorptivity was used to assess the durability of the hardened concrete. The sorptivity
coefficient results
Sorptivity wasofused
the concrete
to assessafter 28 days are
the durability of indicated
the hardenedin Figure 8. It The
concrete. can be noticed
sorptivity
that usingresults
coefficient CBP asoffiller material after
the concrete reduced the sorptivity
28 days are indicatedcoefficient
in Figureof8.the concrete.
It can This
be noticed
is due
that to the
using CBPreduction in the pores
as filler material due the
reduced to the use of CBP.
sorptivity An increase
coefficient in the sorptivity
of the concrete. This is
coefficient
due when adding
to the reduction AEA
in the in producing
pores due to theconcrete was also
use of CBP. found. This
An increase indicates
in the that co-
sorptivity the
Minerals 2022, 12, 159 use of CBP as filler material enhanced the durability of the concrete.
efficient when adding AEA in producing concrete was also found. This indicates that In contrast, adding
the
10 of 17
AEA
use ofdecreased it. This
CBP as filler is consistent
material enhanced with
the(Abd Elrahman
durability et al.,
of the 2020 [23]),
concrete. who found
In contrast, that
adding
a greater
AEA AEA content
decreased it. This leads to a higher
is consistent withsorptivity coefficient.
(Abd Elrahman et al., 2020 [23]), who found that
a greater AEA content leads to a higher sorptivity coefficient.
1.10
Sorptivity coefficient (kg/m2hr0.5)

1.05
1.00
0.95
0.90
0.85
0.80
0.75
0.70
0.65
0.60

Figure
Figure 8.
8. Sorptivity
Sorptivity coefficient.
coefficient.

5.2.6. Porosity
5.2.6. Porosity
The concrete porosity
The concrete porosity was
was measured
measured using
using helium
helium pycnometry.
pycnometry. Figure
Figure 99 shows
shows the
the
concrete porosity
concrete porosity at
at 91
91 days.
days. The
The porosity
porosity of
of MF0
MF0 atat 91
91 days
days was
was 21.54%. It decreased
21.54%. It decreased
when increasing the CBP content. It reached 19.46% in MF30. This could be due to the
when increasing the CBP content. It reached 19.46% in MF30. This could be due to the
denser microstructure that was created by using CBP as a filler material. The utilization
of CBP fills the voids and decreases the porosity. For mixes prepared with AEA, the po-
rosity increased with increasing the AEA content. This may be because the AEA produces
air bubbles in the hardened concrete. The porosity reached 25.08% in MF30-1 when using
 Figure 8. Sorptivity coefficient.

5.2.6. Porosity
The concrete porosity was measured using helium pycnometry. Figure 9 shows the
Minerals 2022, 12, 159 10 of 17
concrete porosity at 91 days. The porosity of MF0 at 91 days was 21.54%. It decreased
when increasing the CBP content. It reached 19.46% in MF30. This could be due to the
denser microstructure that was created by using CBP as a filler material. The utilization
denser
of CBP microstructure thatdecreases
fills the voids and was createdtheby using CBP
porosity. Foras a filler
mixes material.with
prepared TheAEA,
utilization
the po- of
CBP fills the voids and decreases the porosity. For mixes prepared with AEA,
rosity increased with increasing the AEA content. This may be because the AEA produces the porosity
increased
air bubbleswith increasing
in the hardenedthe AEA content.
concrete. This may
The porosity be because
reached 25.08% intheMF30-1
AEA produces
when using air
bubbles in the hardened concrete. The porosity reached
an AEA with a 1% weight ratio in cementitious materials. 25.08% in MF30-1 when using an
AEA with a 1% weight ratio in cementitious materials.

30

25

20
Porosity (%)

15

10

0
MF0 MF10 MF20 MF30 MF30-0.25 MF30-0.5 MF30-0.75 MF30-1

Figure 9. Concrete porosity.

Figure 9. Concrete porosity.
5.3. Microstructural Investigations
5.3. Microstructural
5.3.1. Investigations
Scanning Electron Microscopy (SEM)
5.3.1.Useful
Scanning Electron Microscopy
information (SEM) microstructure can be observed from SEM.
about the concrete
The effect
Useful information about the concrete has
of using CBP as a filler material been studied.
microstructure canThe SEM micrographs
be observed from SEM.of
concrete produced by using 0% CBP as filler material (MF0) and concrete produced
The effect of using CBP as a filler material has been studied. The SEM micrographs of by
using 30%
concrete CBP as filler
produced material
by using 0% CBP(MF30) after material
as filler 91 days are shown
(MF0) and in Figureproduced
concrete 10a,b. Pores
by
with a diameter of about 30 µm were observed in the MF0 sample, while no pores were
observed in the MF30 sample. The micrograph of MF30 shows a denser concrete structure
than that of MF0. This is because using CBP reduces the pores.
To study the effect of the AEA, selected samples of MF30, MF30-0.5, and MF30-1 were
analyzed using SEM. The SEM micrographs of the mixes MF30, MF30-0.5, and MF30-1 at
91 days are shown in Figure 10b–d, respectively. Figure 10b shows that MF30 has a dense
concrete structure. A large number of air-entrained voids with a diameter ranging from
3 to 6 µm can be observed in Figure 10c. These air voids are small, well-separated, and not
connected. Larger pores with a diameter between 150 and 200 µm can be seen in Figure 10d.
These larger pores were created from small collapsing air-entrained voids were created by
the addition of the AEA.

5.3.2. X-ray Diffraction (XRD)

Table 4 indicates the chemical compositions of the XRD diffraction peaks. The XRD
patterns of concrete mixtures (MF0 and MF30) at 91 days are shown in Figure 11. Quartz
(Q), portlandite (P), calcium silicate (CS), calcium silicate hydrate (CSH), and albite (A)
were the main diffraction peaks in MF0 and MF30. Ettringite (E) diffraction peaks were
found in MF0 and MF30. This may be because of the use of gypsum as an activator in
cement. This may also be due to the reaction of the active alumina in the clay brick. Albite
(A) diffraction peaks were seen in MF0 and MF30. This is because of the reaction between
the silica fume and the clay brick. The quartz diffraction peaks of MF30 were observed
to be higher than those in MF0. This could indicate that the increase in quartz was due
to the use of CBP. Calcium silicate diffraction peaks appeared in MF0 and disappeared in
 with a diameter of about 30 µm were observed in the MF0 sample, while no pores were
observed in the MF30 sample. The micrograph of MF30 shows a denser concrete structure
than that of MF0. This is because using CBP reduces the pores.
To study the effect of the AEA, selected samples of MF30, MF30-0.5, and MF30-1 were
analyzed using SEM. The SEM micrographs of the mixes MF30, MF30-0.5, and MF30-1 at
Minerals 2022, 12, 159 11 of 17
91 days are shown in Figure 10b–d, respectively. Figure 10b shows that MF30 has a dense
concrete structure. A large number of air-entrained voids with a diameter ranging from 3
to 6 µm can be observed in Figure 10c. These air voids are small, well-separated, and not
MF30.
connected. Larger Diffraction
pores peaks of between
with a diameter CSH are found in 200
150 and MF0µmandcan
MF30. Portlandite
be seen in Figurediffraction peaks
in MF0
10d. These larger poreswere
werehigher than
created those
from in collapsing
small MF30. Thisair-entrained
is due to thevoids
activewere
silica in the clay brick,
cre-
whichof
ated by the addition reacts with the portlandite (CH) and produces more CSH.
the AEA.

(a) MF0 (b) MF30

(c) MF30-0.5 (d) MF30-1

Figure 10. SEM images
Figure of
10.concrete. (a) MF0,
SEM images (b) MF30,
of concrete. (a)(c) MF30-0.5,
MF0, (d) (c)
(b) MF30, MF30-1.
MF30-0.5, (d) MF30-1.

5.3.2. X-ray Diffraction (XRD)

Table 4. XRD diffraction peaks.
Table 4 indicates the chemical compositions of the XRD diffraction peaks. The XRD
Compound
patternsName Chemical
of concrete mixtures (MF0 and MF30)Formula
at 91 days are shown in FigureICCD Code *
11. Quartz
(Q), portlandite
Albite (A) (P), calcium silicate (CS), calcium
NaAlSi 3 O8 silicate hydrate (CSH), and1616-083-01
albite (A)
Quartz (Q)
were the main diffraction peaks in MF0 and MF30. SiO 2 0539-083-01
Ettringite (E) diffraction peaks were
Ettringite,
found syn (E) and MF30. This may
in MF0 Ca6 Albe
2 (SO 4 )3 (OH)12
because of·26H O of gypsum as an activator
the 2use 1451-041-00
in
Portlandite, syn (P) Ca(OH)2 1481-044-00
cement. This
Calcium silicate (CS)
may also be due to the reaction of
Ca3 SiO5
the active alumina in the clay brick. Albite
0739-055-00
(A) diffraction
Calcium silicate peaks were seen in MF0
hydrate (CSH) Ca2and
SiO4MF30.
·0.35H2This
O is because of the reaction between
0306-033-00
the silica fume *and the clay brick. The quartz diffraction peaks of MF30 were observed to
ICDD code: International Centre for Diffraction Data code.
be higher than those in MF0. This could indicate that the increase in quartz was due to the
use of CBP. CalciumFiguresilicate11diffraction
illustratespeaks
the XRD appeared in MF0
patterns and disappeared
of concrete mixturesin(MF30,
MF30. MF30-0.5, and
Diffraction peaks MF30-1) at 91 days. Quartz (Q), albite (A), calcium silicate (CS), andincalcium silicate
of CSH are found in MF0 and MF30. Portlandite diffraction peaks
MF0 were higher than those
hydrate (CSH)in were
MF30.theThis is due
main to the active
diffraction silica
peaks in in the clay
these brick, which
mixtures. Diffraction peaks of
reacts with the ettringite
portlandite (E)(CH)
wereand produces
observed more CSH.
in MF30. This is because of the reaction of the clay brick or
the utilization of gypsum as an activator in cement. Portlandite (P) diffraction peaks were
observed in MF30. Albite (A) diffraction peaks were found in MF30, MF30-0.5, and MF30-1.
This may be due to the reaction between the CBP and the silica fume. CSH diffraction
peaks were found in MF30 and MF30-1. Diffraction peaks of calcium silicate are found in
MF30-0.5. It was observed that quartz diffraction peaks in MF30 were higher than those in
MF30-0.5 and MF30-1. MF30 had the lowest diffraction peaks of quartz, which indicates
that quartz was highly consumed in MF30. Quartz diffraction peaks in MF30-0.5 were
higher than those in MF30-1. This indicates that the consumption of quartz in MF30-0.5
was higher than that in MF30-1. This may be due to the air voids created from using the
AEA. The consumption of quartz is related to the AEA content.

Minerals 2022, 12, 159
in MF30-0.5 and MF30-1. MF30 had the lowest diffraction peaks of quartz, which indicates
that quartz was highly consumed in MF30. Quartz diffraction peaks in MF30-0.5 were
higher than those in MF30-1. This indicates that the consumption of quartz in MF30-0.5
was higher than that in MF30-1. This may be due to the air voids created from using the
AEA. The consumption of quartz is related to the AEA content. 12 of 17

Q: Quartz
Q
P: Portlandite

CSH;CS
CS: Calcium silicate

CSH;CS

Q;A;CS
Q E: Ettringite
Q

Q;A
A Q

CS
A A A: Albite
CSH: Calcium
Q;A silicate hydrate

Q;A;CS

Q;A;CS
Q;A;CS

Q;A;CS
A MF0

A;CS
A;CS
Q

Q;A
CS
A A A MF30
Q MF30-0.5

CSH;E
A;E
MF30-1
P;E

A;E

CSH

A;E
QE

CSH

Q;P
Q;A;CSH;P A;E

A;E
E E E A

Q
CSH;CS
A;E;CS

A;E;CS
Q;E;CS
Q

Q;A;E
S;E;C
P;E

A;E

Q;A
E E A;E

A
S

5 10 15 20 25 30 35 40 45 50
2Ɵ (°)
Figure
Figure 11. XRD
11. XRD of concrete
of concrete mixtures
mixtures (MF0,(MF0,
MF30,MF30, MF30-0.5,
MF30-0.5, and MF30-1).
and MF30-1).

Table
5.3.3.4.Thermo-Gravimetric
XRD diffraction peaks.Analysis (TGA)
Materials can undergo
Compound Nameseveral thermal reactions,
Chemical which are related toICCD
Formula weightCodechanges
*
or heat releases. DTG
Albite (A) often shows many weight change reactions,
NaAlSi3O8 such as1616-083-01wa-
the loss of
ter or CO2. In cementitious systems, weight loss up to 600◦ C is generally related to the
Quartz (Q) SiO2 0539-083-01
loss of water, and weight loss above 600 ◦ C is mainly due to the release of CO2. Ettringite
Ettringite, syn (E) Ca6Al2(SO4)3(OH)12·26H2O 1451-041-00
(3CaO·Al2O3 ·3CaSO4 ·32H2O) has a hexagonal prismatic shape. Columns of [Al(OH)6]3− octa-
Portlandite, syn (P) Ca(OH)2 1481-044-00
hedra are linked together by calcium and hydroxide ions ([Ca6AI2 (OH)12]6+[3SO4 2− ·26H2O]6− ),
Calcium silicate (CS) Ca 3SiO5 0739-055-00
and sulfate and water molecules are located on the outer surface of the columns. The water
Calcium
between silicate hydrate
the columns (CSH)
was lost at around 100 ◦ C, andCacontinued
2SiO4·0.35H2O
water loss due to0306-033-00
the hydroxides
* associated
ICDD code:with
International Centre for Diffraction Data code. ◦
the silica occurs at temperatures up to 400 C. A peak associated with the weight
loss due to CO2 is observed between 600 and 750 ◦ C. Calcium silicate hydrate (C-S-H) phases
5.3.3.
showThermo-Gravimetric
water loss over a wide Analysis
range of (TGA)
temperatures (50 to 600 ◦ C) caused by the loss of the
water Materials
present can undergo
in the several
interlayer and thermal reactions,CSH
dehydroxylation. which (Care related
1.5 SH 2 and to weight
CSH changes
1.5 ) diffraction
or heatappear
peaks releases. DTG often
between 50 and 200 ◦many
shows weight
C. Calcium change reactions,
hydroxide (Ca(OH)2)such as thedecomposes
generally loss of waterto
CaO and H20 between 400 and 500 ◦ C. Calcite (CaC03) decomposes to CaO and C02 between
600 and 800 ◦ C [42].
Figure 12 presents DTG and TGA curves for MF0 and MF30 at 91 days. Ettringite (E)
diffraction peaks were found at about 65 ◦ C. The ettringite diffraction peak in MF0 was
lower than that in MF30. This may be due to the reaction of the active alumina in the CBP.
CSH diffraction peaks appeared at about 110 ◦ C and 200 ◦ C. These diffraction peaks in
MF30 were higher than those in MF0. This is because of the pozzolanic reaction of the
CBP. Calcium hydroxide (CH) diffraction peaks were observed at about 500 ◦ C. The CH
diffraction peak in MF30 was higher than that in MF0, which indicates that was produced
from the reaction of the CBP. Incorporating CBP as filler material increased the CH and
CSH diffraction peaks as a result of its pozzolanic reaction.
 The DTG and TGA curves for MF30, MF30-0.5, and MF30-1 at 91 days are shown in
Figure 12. Ettringite (E) diffraction peaks were observed at 65 °C. Diffraction peaks of CSH
were found at about 110 °C and 200 °C. CH diffraction peaks could be seen at about 500
°C. All of these diffraction peaks in MF30 were higher than those in MF30-0.5 and MF30-
Minerals 2022, 12, 159 1. From the figure, it is clear that using the AEA reduced the diffraction peaks of CH 13 and
of 17
CSH.

100 0.0

98 (b)
CH C
-0.1
96
(a)
94
-0.2

DTG (mg/min)
92
TGA (%)

90 -0.3
CSH
88
-0.4
86
E: Ettringite
84
CSH: Calcium silicate hydrate -0.5
E MF0 MF30
82 CH: Calcium hydroxide
MF30-0.5 MF30-1 C: Calcite
80 -0.6
0 200 400 600 800 1000

Temp.(°C)

Figure 12. (a) TGA and (b) DTG curves for MF0, MF30, MF30-0.5, and MF30-1.
Figure 12. (a) TGA and (b) DTG curves for MF0, MF30, MF30-0.5, and MF30-1.
The DTG and TGA curves for MF30, MF30-0.5, and MF30-1 at 91 days are shown in
Figure 12. Ettringite (E) diffraction peaks were observed at 65 ◦ C. Diffraction peaks of
CSH were found at about 110 ◦ C and 200 ◦ C. CH diffraction peaks could be seen at about
500 ◦ C. All of these diffraction peaks in MF30 were higher than those in MF30-0.5 and
MF30-1. From the figure, it is clear that using the AEA reduced the diffraction peaks of CH
and CSH.

5.3.4. Mercury Intrusion Porosimetry (MIP)

The effect of using CBP as filler material on the pore size distribution of the concrete
was investigated by using MIP. The average pore diameter was 0.0221 µm in MF0 and
0.0193 µm in MF30, which indicates that the utilization of CBP as filler material in concrete
decreases the diameters of the pores in concrete. The cumulative and incremental pore
volume curves for MF0 and MF30 at 91 days are presented in Figure 13. From the curves, it
can be observed that the pores in MF30 were smaller than those in MF0. The pores may
be classified as gel pores, which have diameters less than 0.01 µm, capillary pores, which
have diameters ranging from 0.01 µm to 10 µm, and air voids, which have diameters up
to 10 µm [43]. The pore size distribution of concrete mixtures (MF0 and MF30) at 91 days
is shown in Figure 14. The use of the CBP as filler material decreased the pore size as the
ratios of gel pores in MF30 appeared to be higher than those in MF0. However, the ratios of
capillary pores and air voids in MF30 were less than those in MF0. This proves that the use
of CBP as filler material fills the pores and decreases their diameters.
Minerals
Minerals 2022,
2022, 12,
12, 159
159 15
14of
of17
17

0.11 0.006
MF0
0.1 MF30
(a)

Incremental pore volume (mL/g)

0.09 MF30-0.5 0.005

Cummulative pore volume (mL/g)

MF30-1
0.08
0.004
0.07

0.06
0.003
0.05

0.04 (b)
0.002
0.03

0.02 0.001
0.01

0 0
0.001 0.01 0.1 1 10 100
Pore diameter (µm)

Figure
Figure 13.
13. (a)
(a) Cumulative
Cumulativeand
and(b)
(b) incremental
incrementalpore
porevolume
volumecurves
curvesof
ofconcrete
concretemixes
mixes(MF0,
(MF0,MF30,
MF30,
MF30-0.5, and MF30-1).
MF30-0.5, and MF30-1).

90

80
Pore size distribution (%)

70

60
MF0
50
MF30
40
MF30-0.5
30
MF30-1
20

10

0
Gel pores Capillary pores Air voids

Figure 14. Pore size distribution of MF0, MF30, MF30-0.5, and MF30-1.
Figure 14. Pore size distribution of MF0, MF30, MF30-0.5, and MF30-1.
The influence of adding an AEA in concrete on the pore size distribution of the concrete
was studied
6. Conclusions using MIP. The average pore diameter was 0.0193 µm in MF30, 0.0218 µm
in MF30-0.5, and 0.0249 µm in MF30-1, which indicates that adding an AEA in concrete
The effects of using CBP as filler material and adding an AEA in crushed clay brick
increases the diameters of the pores in the concrete. The diameters of the pores increase
concrete were investigated. The following conclusions were obtained from the results:
with the increase in the AEA content. The cumulative and incremental pore volume curves
1. The usemixtures
of concrete of CBP as a fillerMF30-0.5,
(MF30, material and
increases the at
MF30-1) concrete
91 daysworkability.
are indicated It in
also caused
Figure 13.
The pores in MF30 were found to be smaller than those in MF30-0.5 and MF30-1. ther-
an increase in the concrete dry density, compressive strength, UPV values, and This
mal conductivity
indicates that adding AEA withincreases
the increase
the in the
size ofCBP content
the pores. aspores
The it filled
in the pores and
MF30-0.5 there-
ere smaller
than those in MF30-1. The pores increased with increasing the AEA content. Figure an
fore enhanced the mechanical and durability properties of the concrete. There was 14
observed
presents decrease
the pore in the concrete
size distribution porosity
of MF30, when and
MF30-0.5, the CBP wasatused
MF30-1 as filler
91 days. Thematerial.
ratios of
Microstructural
gel pores in MF30 were investigations
found to be (SEM,
higherXRD, TGA, in
than those and MIP) proved
MF30-0.5 that using
and MF30-1. CBPalso
It was as
founda filler material
that the ratios decreases
of gel porestheincapillary
MF30-0.5pores
wereand
less air
thanvoids
thoseininthe concrete;
MF30-1. this is due
A decrease in
Minerals 2022, 12, 159 15 of 17

the gel pores was observed when using the AEA in concrete, and this decrease increased
with the increase in AEA content. From the figure, it can be noted that the ratios of capillary
pores and air voids in MF30 were found to be less than those in MF30-0.5 and MF30-1.
This indicates that the addition of an AEA in concrete increases the capillary pores and air
voids. The capillary pores and air voids in MF30-0.5 were smaller than those in MF30-1.
This indicates that the utilization of an AEA in concrete increases the capillary pores and
air voids. An increase in the capillary pores and air voids was found with the increase in
AEA content. This proves that increasing the AEA content increases the diameters of the
pores as the small pores collapse and become bigger.

6. Conclusions
The effects of using CBP as filler material and adding an AEA in crushed clay brick
concrete were investigated. The following conclusions were obtained from the results:
1. The use of CBP as a filler material increases the concrete workability. It also caused an
increase in the concrete dry density, compressive strength, UPV values, and thermal
conductivity with the increase in the CBP content as it filled the pores and therefore
enhanced the mechanical and durability properties of the concrete. There was an
observed decrease in the concrete porosity when the CBP was used as filler material.
Microstructural investigations (SEM, XRD, TGA, and MIP) proved that using CBP
as a filler material decreases the capillary pores and air voids in the concrete; this
is due to its filling ability and pozzolanic activity, which caused an increase in the
CSH content.
2. Adding an AEA in concrete increases its workability. However, it decreases the
concrete dry density, compressive strength, UPV values, and thermal conductivity
when the AEA content is increased in the concrete due to the created voids. These
voids negatively affect the mechanical and durability properties of concrete but
improve its thermal properties. An increase was also found in the concrete porosity
while increasing the AEA content. Microstructural investigations (SEM, XRD, TGA,
and MIP) proved that adding an AEA in concrete decreases the formation of CSH
and increases the capillary pores and air voids, and this is related to the amount of
the AEA.

Author Contributions: H.A.-k.; Conceptualization, funding acquisition, writing, and supervision,

M.M.A.; Data curation, formal analysis, methodology, writing, resources, M.G.M.; Conceptualization,
supervision, review, M.A.E.; Conceptualization, methodology, formal analysis, writing review and
editing, supervision. All authors have read and agreed to the published version of the manuscript.
Funding: This research received no external funding.
Acknowledgments: The authors express their sincere gratitude for the financial support provided by
the Deanship of The Scientific Research University of Jordan.
Conflicts of Interest: The authors declare no conflict of interest.

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