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Study of fired clay bricks with coconut shell waste as a renewable pore-forming agent:
Technological, mechanical, and thermal properties

Zineb Moujoud, Achraf Harrati, Ahmed Manni, Amine Naim, Abdeslam El Bouari,
Omar Tanane
PII: S2352-7102(23)00286-3
DOI: https://doi.org/10.1016/j.jobe.2023.106107
Reference: JOBE 106107

To appear in: Journal of Building Engineering

Received Date: 28 November 2022

Revised Date: 12 February 2023
Accepted Date: 12 February 2023

Please cite this article as: Z. Moujoud, A. Harrati, A. Manni, A. Naim, A. El Bouari, O. Tanane, Study
of fired clay bricks with coconut shell waste as a renewable pore-forming agent: Technological,
mechanical, and thermal properties, Journal of Building Engineering (2023), doi: https://doi.org/10.1016/
j.jobe.2023.106107.

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Study of fired clay bricks with coconut shell waste as a renewable pore-forming
agent: Technological, mechanical, and thermal properties

Zineb Moujoud a,*, Achraf Harrati a, Ahmed Manni a, Amine Naim a, Abdeslam El Bouari a,
Omar Tanane a

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Laboratory of Physical Chemistry, Materials and Catalysis, Faculty of Sciences Ben M’Sick,
Hassan II University of Casablanca, Morocco

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* Corresponding author email: zineb.moujoud-etu@etu.univh2c.ma ;

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Phone number: +212637953708

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Abstract
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In the present work, coconut shell powder (CSP) is explored as a pore-forming agent in the
manufacturing of fired clay bricks. The bricks were produced by varying the amount of CSP (0, 10,
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20, and 30 wt.%), and fired at different temperatures (900, 1000, and 1100 °C). Mineralogical,
physical, mechanical, and thermal conductivity tests were performed to evaluate the properties of
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the elaborated bricks. It is found that the addition of CSP does not influence the mineralogy of the
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bricks. Besides, mechanical strength, bulk density, and firing shrinkage increase with sintering
temperature and decrease with increasing CSP content, while water absorption and porosity
decrease with temperature and increase with CSP addition. Otherwise, the combination of firing at
1100 °C with 30 wt.% addition of CSP in clay brick provides lower thermal conductivity (0.37
W.m-1.K-1), while maintaining adequate tensile strength (9.88 MPa). This finding suggests the reuse
of CSP as a pore-forming agent to elaborate bricks with thermal insulating character.

Keywords: Fired clay bricks; Coconut shell waste; Pore-forming agent; Thermal conductivity

1. Introduction
Energy conservation in the building sector has become one of the most important issues at the
moment [1]. It was reported that one-third of the world’s energy consumption is consumed in
buildings [2], while 50% of this energy is lost; due to the low thermal insulation of building

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materials [3]. Actually, building materials have been widely developed to improve thermal
insulation and optimize the energy performance of buildings [4]. Within the sustainability context,
using ecological, lightweight, and low-cost thermal insulation materials have recently emerged.
Fired clay brick is one of the most widely used building materials in the world [5], due to its
remarkable physical and mechanical properties, especially its durability, fire resistance and strength
[6,7]. Indeed, fired clay brick relies on a simple manufacturing process and the use of cheap and
abundant raw materials: a mixture of clay, silica sand, feldspars, and water [8]. The approximate
annual production of bricks in the world is about 1391 billion units, which is expected to increase
continuously due to the increased demand in the construction sector [9]. In fact, fired bricks have a

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limited thermal conductivity value, usually about 1.0±0.4 W.m-1.K-1 depending on the raw materials
and the firing process, which means a significant heat loss through the house walls [10]. However,

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this unfavorable property can be solved by introducing pores into the bricks. When pores are

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created, the thermal conductivity and density of the bricks are reduced [10–12]. This can be
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achieved by introducing holes extending through the brick as in the case of a perforated brick or by
incorporating particles as pore-forming agents in the clay mixture [13,14]. The latter method is
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widely used by the bricks industry [14]. When a pore-forming agent is used, the organic matter
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burns during the firing process and leaves behind pores, thus improving the thermal insulation
properties of the brick [10,11,15,16]. However, the choice of the pore-forming agent depends on its
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physico-chemical characteristics, its availability, and its ability to combust completely [14].
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Therefore, with ecological awareness, researchers are increasingly interested in using various
wastes (agricultural, industrial, and urban) as pore-forming agents in fired brick making [14]. The
use of wastes in brick industry could have environmental and energetic advantages, on the one
hand, by valorizing wastes that are not widely used or usually end up in landfills and, on the other
hand, by reducing the energy needed to produce bricks due to their high calorific value [17–19].
Upon a review of the literature, it was found that using wastes with large amounts of organic matter
can promote more pore formation in the clay body during the firing process due to the chemical
degradation and the corresponding gas release [14,20,21]. Among organic wastes, many agricultural
and industrial co-products have been used as pore-forming agents due to their wide availability and
low costs, such as waste tea [11], rice husks [22,23], corn cob [16,24], cigarette butts [15,25], olive
mill waste [26,27], paper pulp [20], and sawdust [28]. Furthermore, the content and the particle size
of the pore-forming agent influence the thermal conductivity of bricks. Aouba et al. [29]

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investigated the use of olive stone flour (OSF) with a particle size of 50 μm and wheat straw (WS)
with a particle size of less than 500 μm as pore-forming agents. The results showed that the lowest
thermal conductivity value was obtained for 7 wt.% WS (∼0.30 W.m-1.K-1) compared to OSF
(∼0.39 W.m-1.K-1) when 8 wt.% is incorporated. Similarly, Ahmad et al. [30] revealed a decrease in
the thermal conductivity of bricks by 27%-68% and by 48%-92% with an increase in coal and
wheat husk content from 5 to 50 wt.%, respectively. This indicates the influence of the content and
the particle size of the pore-forming agent on the total porosity and thermal conductivity.
Nevertheless, increasing the content and particle size of the pore-forming agent is undesirable due
to their negative effect on the strength and physical properties of bricks [30]. Therefore, the content

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and particle size of the pore-forming agent must be controlled.
In this study, organic coconut shell waste is investigated as a pore-forming agent in fired bricks.

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The coconut tree, a member of the palm tree family (Arecaceae), is grown in more than 100

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countries. The global production of coconut is about 250-300 million tons for the year 2018 [31].
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The coconut shell, which represents 15-20% of the coconut, is a hard lignocellulosic waste that
takes a long time to decompose [32]. Coconut shell is commonly discharged by farmers and
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processors as abundant agro-industrial waste or open burned, creating serious problems in the local
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environment [33]. Therefore, different approaches to recycle coconut shell waste have been
proposed, such as charcoal briquettes production [34,35], and activated carbon production [36,37].
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In addition, the use of coconut shell waste in the building sector has been investigated. Gunasekaran
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et al. [38] recommended using coconut shell as alternative coarse aggregates in the production of
hollow blocks, which can reduce the self-weight and material transportation and handling costs.
Another study confirmed the use of coconut shell as lightweight aggregates for concrete production
in practice without any hesitation given their durability properties [39]. However, the amount of
coconut shell waste reused is less compared to its availability. Therefore, recycling coconut shell
powder (CSP) as a pore-forming agent in bricks production is a viable way to manage this waste
and minimize the volume sent to landfill. CSP contains a high volatile matter content (∼80 wt.%)
with low compositions of ash (∼2 wt.%), and carbon and oxygen are the major elements [40–42].
When burnt, CSP leads to the emission of CO2 which can create pores in the brick body. On the
other hand, local availability, renewable nature, and low cost are the main reasons for using CSP as
a pore-forming agent in this work.

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To the authors’ knowledge, there is no study on using CSP as a pore-forming agent. This can be
valuable to explore its performance as a pore-forming agent compared to other currently used pore-
forming agents. In this study, the effects of CSP incorporation and the firing temperatures on the
technological properties (i.e., linear shrinkage, porosity, water absorption, and bulk density),
mechanical strength (i.e., diametral compression strength), microstructure, and thermal conductivity
of the developed bricks were investigated. The results obtained in this study are intended to help
future research to pay attention to this waste and to promote its economic and environmental use.

2. Materials and methods

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2.1. Raw materials
The red clay sample used in this study to prepare the fired bricks was collected from the Safi region

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(Safi, Morocco). Locally, this clay is used for making pottery. The selected clay was crushed and

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stored in the laboratory under controlled conditions (T=25 °C, Humidity = 50%). Similarly, coconut
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shell waste was taken from local vendors in Casablanca-Morocco. The coconut shell was oven
dried, ground in a ball mill, and sieved to obtain fine powder (CSP) before being used as a pore-
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forming agent in the fired specimens.

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2.2. Methods
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The methodological approach adopted in this study can be resumed as follow: the first step consists
of preparation and characterization of the raw material (i.e., XRF, CHNS-O, XRD, IR and
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DTA/TG). The second step of the process consists in preparing the brick samples incorporating
varying percentages of CSP at 0%, 10%, 20%, and 30% by weight. Three specimens were prepared
for each level of CSP addition. Finally, many tests were done on the elaborated bricks (i.e., XRD,
SEM, linear shrinkage, porosity, water absorption, bulk density, thermal conductivity and diametral
compression strength) to investigate and evaluate their properties. For each test, the obtainedresults
present the average of three values.

2.2.1 Characterization of raw materials

The chemical composition of the raw materials was determined by X-ray fluorescence (XRF) using
the Epsilon 4 instrument. The content of H, O, S, and C in coconut shell powder was measured by a
PerkinElmer EA2400 series II CHNS-O Elemental Analyzer. N detection limit was 1.20%. The
particle size distribution of the raw materials was carried out using the Malvern Mastersizer 2000.

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X-ray diffraction (XRD) of the raw and elaborated materials was carried out using a BRUKER D8
ADVANCE diffractometer. XRD experiments were achieved in step-scan mode from 10° up to 65°
(2θ). Fourier Transform infrared spectroscopy (FTIR) using a Bruker Tensor 27 FTIR spectrometer
operating in the range 4000-400 cm-1. Thermal analyses (DTA-TG) were carried out using a
LABSYSEVO multichannel instrument apparatus. The scanning was carried out at different ranges
of temperatures depending on the phenomena appearing in the studied material (from 23 °C to 1000
°C for the clay sample, and to 600 °C in the CSP) with a heating rate of 5 °C/min under air
atmosphere.

2.2.2 Manufacturing of bricks

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The raw materials (red clay and coconut shell waste), separately, are oven dried at 105 °C for 24h,

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ground in a ball mill, and sieved to a particle size < 63 µm. The bricks were manufactured through
the dry-pressing technique. The coconut shell powder (CSP) was added to the red clay at 0, 10, 20,

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and 30% by weight, and re-crushed for 15 minutes to obtain homogeneous powders. The powders
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were moistened with a sprayer to the limit of 4-6% water. Next, the moistened powders were
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pressed using a hydraulic press of 40 MPa in a cylindrical steel mold to prepare specimens of 50
mm in diameter and 25 mm in thickness. The samples were oven-dried at 105 °C for 24 h to remove
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excess moisture that might cause cracking during the firing process. Finally, the samples were fired
at 900, 1000, and 1100 °C in the furnace with a heating rate of 5 °C/min and then naturally cooled
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in the furnace.
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2.2.3 Characterization of elaborated bricks

The loss on ignition (LOI) of the brick samples was determined by measuring the mass loss of the
sample between the drying and sintering stages. The following equation was used [43]:
𝑀𝑑 − 𝑀𝑓
LOI(%) = × 100 (1)
𝑀𝑑
where 𝑀𝑓 is the sample mass after firing, and 𝑀𝑑 is the sample mass after oven drying.
For the diametrical shrinkage, the diameter of the specimens was measured before and after the
sintering step using a caliper (accuracy ±0.01 mm). The resulting values are used to calculate the
diametrical shrinkage according to ASTM C326-09 [44]:
𝐷𝑑 − 𝐷𝑓
Diametrical shrinkage (%) = × 100 (2)
𝐷𝑑
where 𝐷𝑓 is the sample diameter after firing, and 𝐷𝑑 is the sample diameter after oven drying.

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A procedure based on ASTM C373-88 standard [45] was used to measure the water absorption,
bulk density, and apparent porosity of the bricks by the following formulas:
𝑀𝑤𝑒𝑡 − 𝑀𝑑𝑟𝑦
Water absorption (%) = × 100 (3)
𝑀𝑑𝑟𝑦
g 𝑀𝑑𝑟𝑦 g
Bulk density ( 3 ) = × water density ( 3 ) (4)
cm 𝑀𝑤𝑒𝑡 − 𝑀𝑠𝑢𝑠𝑝𝑒𝑛𝑑𝑒𝑑 cm
𝑀𝑤𝑒𝑡 − 𝑀𝑑𝑟𝑦
Apparent porosity (%) = × 100 (5)
𝑀𝑤𝑒𝑡 − 𝑀𝑠𝑢𝑠𝑝𝑒𝑛𝑑𝑒𝑑
where 𝑀𝑑𝑟𝑦 is the constant mass of the specimen after drying at 105–115 °C, 𝑀𝑤𝑒𝑡 is the mass of
the specimen after water saturation and 𝑀𝑠𝑢𝑠𝑝𝑒𝑛𝑑𝑒𝑑 is the mass of the water-saturated sample.

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The mechanical properties of the fired samples were assessed using an indirect tensile test. The

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Brazilian Test (diametral compression) was used to measure the tensile strength of the specimens

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(ASTM C496 [46]). This test consists of applying a load vertically on the diameter of a rather thin
disk (typically 50 mm in diameter and 10 mm in thickness). The tensile strength σr (MPa) is given
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by the following equation [47]:
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2×𝑃
σr (MPa) = (6)
𝜋×𝐷×𝑡
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where 𝑃 is the maximum applied load (N), 𝐷 is the diameter (mm), and 𝑡 isthe thickness of the
sample (mm).
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Thermal conductivity of brick samples was performed according to the standard ASTM C177 [48]
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using a Thermal Conductivity Analyzer type λ-Meter EP500e. This technique consists in applying
variable heat flux in a block comprising a sample taken between two plates. The measurement is
carried out at three temperatures 10, 25, and 40 °C, and under a pressure of 2500 Pa for each
temperature.
The surface morphology of the elaborated bricks specimens was observed using Hirox SH-4000M
scanning electron microscope at an accelerating voltage of 10 kV and using a secondary electron
detector (SE).

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3. Results and discussion

3.1. Characterization of raw materials

3.1.1. Chemical composition (XRF, CHNS-O)

The chemical composition of the red clay is shown in Table 1. The results reveal important contents
of silica and alumina 51.69% and 20.04% respectively, with a silica/alumina ratio ≈ 2.58 which
explains the high content of quartz in the clay sample. A relatively high content of Fe2O3 (5.35%)
makes it appropriate for dark red coloring products (%wt of Fe2O3 > 3%) [49], and responsible for
the reddish color of the brick body after high-temperature treatment. The content of alkaline earth

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oxides CaO and MgO are low; 3.20% and 2.86% respectively, which explains the relatively low

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carbonate content. The high percentage of K2O (4.44%) explains the richness of the red clay in
illitic clay minerals and also the presence of potassium feldspars responsible for the decrease of the

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melting temperature of the material at high temperatures. The loss on ignition content (12.00%) is
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related to the elimination of adsorbed and structural water as well as the decomposition of organic
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matter and carbonates. The rest of the oxides (Na2O, P2O5, TiO2) are present in insignificant
contents (≈ 0.43%).
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Table 1. XRF analysis of red clay and CSP after combustion (Ash state)
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Oxide content
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SiO2 Al2O3 Fe2O3 CaO MgO K2O Na2O P2O5 TiO2 LOI(*)
(wt%)
Safi clay 51.69 20.04 5.35 3.20 2.86 4.44 0.12 0.18 0.13 12.00
CSP (Ash state) 48.45 15.61 13.60 0.56 16.21 0.87 0.44 0.29 0.01 -
(*): Loss on ignition obtained after calcination at 1000 °C for 1h

Table 2 displays the chemical composition of the coconut shell powder (CSP) in its raw state by
CHNS-O analysis. The CSP is composed totally of organic matter 48.4% C, 44.59% O, 6.8% H,
with low traces of N, S, and Cl. Moreover, the ash content after the combustion of the raw CSP is
about 1.8% of the total mass. XRF analysis of dry ash of CSP (Table 1) demonstrates the
predominant of SiO2 (48.45%) along with MgO (16.21%), Al2O3 (15.61%), and Fe2O3 (13.60%),
with some negligible traces of other oxides. The obtained results are following those found in the
literature [40,50].

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 Table 2. CHNS-O analysis of the coconut shell powder (CSP) in the raw state

Elements Composition (%wt)

C 48.4
H 6.8
N 0.13
O 44.59
Cl 0.07
S <0.01

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3.1.2. Particle-size distributions

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In bricks manufacturing, it is commonly known that the particle size of the raw materials used

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influences the porosity after the sintering process. For this reason, Fig. 1 shows the particle size
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distribution for the red clay and coconut shell powders. The analyzed powders show a bimodal and
unimodal shape in the range of 0.1-59 µm and 0.1-76 µm for the clay and CSP samples,
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respectively. The curve shows that the CSP was ground to a fineness that is close to that of the red
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clay powder. According to the results, the particle size corresponding to cumulative volume
percentages below 10, 50 and 90% are 1.99, 10.7 and 32.9 µm, and 3.2, 10.5 and 30.5 µm for red
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clay and CSP, respectively. On closer observation, it can be deduced that the majority of the
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particles are smaller than 33 µm for both clay and CSP samples. These results confirm that the
powders used are very rich in fine fractions which help to minimize the pore size without the
appearance of macropores or/and cracks.

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Fig. 1. Particle size distribution of (a) Red clay and (b) Coconut shell powder
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3.1.3. Mineralogical composition (XRD)

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X-ray diffraction (XRD) patterns of red clay and coconut shell powder are shown in Figure 2. In
Fig. 2-a, it was observed that quartz (Q) is the main mineralogical phase in clay. However, other
mineralogical phases revealed in clay such as dolomite (D), calcite (C), feldspar (F), illite (I),
kaolinite (K), and chlorite (Ch) offering favorable properties for ceramic use.
As shown in Fig. 2-b, the most important diffractions in coconut shell waste are observed by three
crystalline peaks at the following angles: 2θ = 14.84°, 22.67°, and 34.23° represent the plane (120)
(002) (123) respectively, which corresponds to the planar crystallographic family of cellulose [51].

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Fig. 2. XRD diffractograms of raw materials: (a) Red clay and (b) Coconut shell powder

3.1.4. FTIR characterization

The FTIR spectrum of the raw materials was recorded in the range of 4000-400 cm-1 as shown in
Fig. 3. The assignments of the bands were based on literature data. From the FTIR spectrum of red
clay in Fig. 3-a, the presence of absorption bands at 3620 cm−1 can be attributed to the asymmetric
stretching of structural hydroxyl groups OH. The broad band located at 3416 cm−1 is assigned to the
stretching vibration of adsorbed water. The band around 1632 cm−1 is assigned to OH bending
vibration of adsorbed water in the structure of silicate [49]. The band observed at 1042 cm−1 is
attributed to Si–O stretching [52]. The bands in 694 cm−1 and 472 cm−1 are attributed to Si–O
stretching and Si–O bending modes, respectively [52]. Absorption at 535 cm−1 is related to Si-O-Al,
where the Al is in octahedral coordination [53].

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From the FTIR spectrum of coconut shell powder shown in Fig. 3-b, the peak at about 3404 cm−1 is
due to hydrogen-bonded O–H stretching. The peak at 2927 cm−1 is due to the C-H stretching that
causes vibrations of CH, CH2, and CH3 groups [42]. The peak at 1728 cm−1 is due to the carbonyl
group C=O stretching [54]. The peak at 1636 cm−1 is reflected to N-H bending in the primary amine
group presents in the sample. The peak at 1512 cm−1 is due to the stretching vibrations in aromatic
structure C=C [42]. The peak at 1245 cm−1 represents Si–CH2 stretching in alkane or C–C plus C–O
plus C=O stretching and deformation bands in cellulose and lignin [42,55]. The absorbance peak at
1052 cm−1 is assigned to C–O deformation in secondary alcohol and aliphatic ether [55]. A peak at
898 cm−1 is attributed to the C–H in plan deformation plus C–O deformation in primary alcohol

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[55]. The peak at 1461 cm−1 corresponds to the C-H bending of CH3 groups. The peak at 1376 cm−1
is reflected to the symmetric and asymmetric bending of CH3 groups. The peak at 1103 cm−1 is due

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to the C–N stretching [56]. The peaks at 597 cm−1 and 830 cm−1 contributed to the C-H stretching
vibrations [54].
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Fig. 3. FTIR spectrum of raw materials: (a) Red clay and (b) Coconut shell powder
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3.1.5. Thermal analysis (DTA-TG)

The DTA-TG curves of the raw materials are shown in Fig. 4. Fig. 4-a shows four peaks for the red
clay. The first endothermic peak below 100 °C represents the evaporation of absorbed water
molecules. The second endothermic peak 514 °C is due to the desorption of structural water (i.e.,
dehydroxylation of kaolinite and illite) [49]. The third endothermic peak at 694 °C is due to the
reversible α/β quartz transition. Finally, the small peak at 943 °C which does not correspond to a
loss of mass is reflects the formation of spinel structure and/or primary mullite.
During the heating process of the clay sample, two significant stages in weight loss percentage were
detected: at 25–200 °C with 3.34 % and 400–700 °C with 8.75%, respectively. At 25–200 °C, the
weight loss is mainly attributed to the rapid desorption of adsorbed water and interlayer water in the
clay surface and interlayer space. At the temperature range of 400–700 °C, the weight loss is mainly

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due to the combustion of organic matter and the dissipation of structural water (structural OH
groups). When the temperature reaches 700–1000 °C, the clay mass remains unchanged.
Fig. 4-b presents the DTA-TG curves of coconut shell powder (CSP). The first peak at 64 °C is
related to the elimination of water and other primary volatile substances [40]; where the sample
loses only about 9.41% of its original mass. Furthermore, the CSP presents two degradation steps,
the first observed at 324 °C is explained by the simultaneous decomposition of cellulose,
hemicellulose, and pectin, and the second at 435 °C is related to the decomposition of lignin [40].
The material loses about 88.82% of its original weight, that’s mean is almost totally carbonized.

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Fig. 4. DTA/TG diagrams of raw materials (a) Red clay and (b) Coconut shell powder
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3.1.6. Microstructural observation (SEM)

SEM observations of raw materials (Fig. 5) demonstrate the microstructural aspect of the studied
powders. Fig. 5-a and Fig. 5-b confirm the morphology and fundamental size of the illite clay, the
images show a lath-like shape of the illite grains with a size of less than 5 µm. Agglomerations are
also observed due to the ability of the raw clay to absorb moisture water, which attaches the fine
clay particles together forming agglomerated particles of larger size.
Fig. 5-c and Fig. 5-d show the morphology of the CSP used in this work. As shown, the CSP
appears to be very fine, however, on higher magnifications, it can be seen that the powder consists
of particles with a size of about 60 µm and below. It can be noticed that the CSP appeared to be
small pebble shaped and had a surface containing closed pores due to the presence of volatiles and
other contaminants on the surface [42,57]. In order to be a pore-forming agent, the material must be

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in the form of very fine particles, and the results obtained show that CSP is a good candidate to be
used in the mixture with clay as a pore-forming agent.

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Fig. 5. The morphological aspect of raw materials: (a) and (b) Red clay powder; (c) and (d) Coconut
shell powder

3.2. Characterization of elaborated bricks

3.2.1. Macroscopic aspect of bricks

The appearance of the brick samples in terms of surface color and crack development is shown in
Fig. 6. The color of the brick is essential to classify bricks [58]. The red color is thought to be
caused by iron oxide content after firing at appropriate temperatures [49]. No significant impact of
coconut shell powder incorporation on color is observed [59]. Moreover, no surface defects were
observed in any specimens.

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Fig. 6. Macroscopic aspect of fired clay bricks at 900-1100 °C

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3.2.2. Phase composition of bricks

The X-ray diffraction patterns of the prepared brick mixtures (0, 10, 20, and 30% CSP) fired at 900,
1000, and 1100 °C for 1 h are given in Fig. 7. It can be observed that the primary minerals
composing the studied clay sample (e.g., dolomite, calcite, feldspar, illite, kaolinite, and chlorite)
disappeared after the heat treatment with the appearance of newly formed phases. At 900 °C,
kaolinite (Al2Si2O5(OH)4) is no more observed and transformed into metakaolinite through the
removal of the hydroxyl groups of the silicate lattice above 450 °C [60]. Anorthite (CaAl2Si2O8) is
the first new mineral that appeared at 900 °C and its maximum abundance is observed at 1100 °C.
Anorthite was probably formed by the multistage solid-state reactions between the clay matrix and
carbonate [49,60]. Gehlenite (Ca2Al2SiO7) and spinel (MgAl2O4) were firstly identified at 900 ºC,
and their abundances were noticed at 1100 ºC. Gehlenite is formed by a reaction between calcium

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oxide CaO from calcite and metakaolinite [49]. Spinel is formed by a reaction between magnesia
(MgO) and alumina (Al2O3). The MgO was derived from the dehydroxylation of chlorite and
dolomite minerals and alumina (Al2O3) resulting from the destruction of clay minerals and K-
feldspar [49]. The peaks of orthoclase appeared at 900 ºC and completely disappeared at 1000 ºC.
This is due to their contribution to the formation of the mullite phase [61]. Quartz (SiO2) was the
only primary mineral to be able to resist higher temperatures (up to 1100 °C). The peaks of quartz
are present during all firing temperatures and decreased at higher temperatures due to its dissolution
and/or its conversion into minor amounts of cristobalite [60]. Mullite appeared at all tested
temperatures (900-1100 °C) in small amounts, which could be related to the presence of sufficient

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illite content. After the destruction of illite by hydroxylation, they reacted with quartz and modified
it into mullite [49]. Diopside (CaMgSi2O6) is probably formed from the reaction of CaO, MgO, and

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SiO2 at high temperatures; CaO was probably supplied from calcite and dolomite, however, MgO

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seems to be originated from chlorite and dolomite; its formation was marked mainly by a sharp
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decrease in quartz content [60]. Furthermore, based on the XRD patterns (Fig. 7), the addition of
CSP does not modify the mineralogical composition compared to bricks without additives, which is
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confirmed by the appearance of the same formed phases at all mixtures and sintering temperatures
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[62].
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Fig.7. XRD diagrams of different bricks fired at (a) 900 °C, (b) 1000 °C and (c) 1100 °C
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3.2.3. Technological and mechanical properties of bricks

The weight loss of fired bricks with respect to CSP content is presented in Fig. 8-a. It is well shown
that the firing temperature has less effect on brick weight loss compared with the CSP content. By
increasing the CSP content in the clay mixtures, the weight loss apparently increased. A similar
finding was observed in other studies [12,63–65]. This increase trend of brick weight loss is related
to the departure of water, the combustion of organic matter, and the decomposition of carbonate
minerals present in both clay and CSP [63]. During the firing process below 950 °C, all the organic
matter is volatilized [64]. Typically, brick weight loss results are compatible with thermal results
(DTA-TG) of raw materials (Fig. 4).
Fig. 8-b symbolizes the diametric shrinkage of the CSP incorporated fired bricks between 900 °C
and 1100 °C. The diametric shrinkage increased with the increase in sintering temperature as

22
reported in previous works [12,24,65–67]. This increasing trend of shrinkage may be the
consequence of the formation of liquid-phase and inter-particle cohesion in the bricks during the
firing process [63]. Moreover, it was observed that shrinkage decreased as the amount of
incorporation of CSP increased. This may be related to the distribution and burning of CSP which
cause the existence of residual porosity resulting during the firing process [24]. According to the
literature, firing shrinkage is a significant parameter that affects the brick quality [24,68]. If the
shrinkage is more than 8%, it could increase the risk of cracks and dimensional defects in bricks
[69]. However, it was observed that for CSP incorporated fired bricks, the diametric shrinkage was
below the value of 8%.

of
Apparent porosity is a significant factor affecting the physico-mechanical and thermal properties of
fired bricks [12]. The increase in the porosity decreases the strength and the thermal conductivity

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properties [70]. Fig. 8-c shows that the apparent porosity increases with increasing CSP content.

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This may be attributed to the increase in pore number in the brick structure due to the addition of
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CSP that burned during the firing process. The combustion of the organic matter contained in the
additive leads to the emission of CO2 which gradually releases from the material and creates pores
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in the brick [62]. However, the apparent porosity decreases with increasing sintering from 900 to
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1100 °C. This reduction is associated with the densification and vitrification of the clay bodies at
higher firing temperatures [24,49]. Similar results have been observed in other studies. Making
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bricks with the addition of agricultural waste such as 7 wt.% wheat straw [29], 8 wt.% olive stone
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flour [29], 15 wt.% corn cob [24], and 50 wt.% wheat husk waste [30], increase the porosity by
43.5%, 40.6%, 48%, and 65%, respectively. In the present study, the maximum apparent porosity
value was 52.85% for 30 wt.% CSP content. Considering the literature data, the present
experimental results suggest using CSP as a pore-forming agent in brick manufacturing, thus
increasing the porosity and thermal insulation performance.
Bulk density is strongly influenced by the pores and voids formed in the clay brick structure during
the firing process [30]. As shown in Fig. 8-d, the bulk density value of samples without any
addition was the maximum, while it decreased with increasing CSP content in brick bodies. Similar
findings have been reported in previous studies [12,67,68]. The bulk density correlates inversely
with porosity. The lower bulk density is more noticeable from 30 wt.% CSP content. Pores and
voids are formed in the brick samples due to the almost complete carbonization of CSP, which
eventually results in porous structures and lower bulk densities [62]. Lightweight samples with high

23
porosity could be interesting for thermal or acoustic insulation or for partitions, as recommended by
Njeumen Nkayem et al. [24]. On the other hand, with a constant CSP content, the bulk density
increases with the firing temperature. This is attributed to the formation of vitreous phases helping
to fill the open porosity [24,64].
Water absorption is essential to determine the durability of building materials. The more brick
absorbs water, the less durable it becomes [66]. The results in Fig. 8-e show that the addition of
CSP increases the water absorption of bricks regardless of the firing temperature. This improvement
is expected since the CSP contained in clay bodies is almost completely carbonized during the
firing process, leading to an increase in the open porosity of the brick samples [24,66,71].

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Moreover, the increase in firing temperature leads to a decrease in the water absorption rate of brick
samples. The values obtained at 1100 °C are lower than the others owing to the intense brick

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densification related to the formation of vitreous phases, which leads to a coalescence phenomenon

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of the closing pores [24]. For 10 wt.% addition, the water absorption of bricks fired between 900 °C
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and 1100 °C still lies below the maximum value of 22% required by the ASTM C62 standard [72].
Therefore, according to ASTM C62 [72] standard, the bricks containing 20 wt.% and 30 wt.% CSP
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can be used for negligible weathering conditions. These bricks may be evaluated in insulation
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applications where there is no contact with water. Similar findings have been reported by many
researchers [12,73,74].
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Fig. 8-f reveals that the tensile strength values are significantly degraded when the additive in the
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brick increases from 0 wt.% to 30 wt.%. This decrease can be explained by the increase in pores
due to the combustion of CSP, which results in a considerable decrease in tensile strength [67,75].
Similarly, Monedero et al. [65] revealed that adding agro-industrial waste ashes (exhausted olive
cake and almond shell) decreases the tensile strength of bricks. However, the tensile strength shows
an increasing trend with the firing temperature. The maximum tensile strengths (19.46 MPa and
15.71 MPa) were achieved in bricks with 0 wt.% and 10 wt.% CSP at 1100 °C, respectively. This
enhancement is mainly related to the densification of the clay bodies. This is due to the gradual
formation of anorthite and mullite, which are strong phases contributing to the formation of vitreous
phases helping to fill the open porosity and improve the strength of bricks [67,76]. This is
confirmed by the X-ray pattern (Fig. 7).

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 Fig. 8. Evolution of physical and mechanical properties of brick specimens at 900, 1000 and 1100
°C: (a) LOI (%), (b) Diametric shrinkage (%), (c) Bulk density (g/cm3), (d) Apparent porosity (%),
(e) Water absorption (%) and (f) tensile strength (MPa).

3.2.4. Thermal conductivity of clay bricks fired at 1100 °C

Lower thermal conductivity is beneficial because it reduces the energy consumed for cooling and
heating [15,16]. Based on the mechanical results, the thermal performance of bricks fired at 1100

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°C is presented in Fig. 8. It is shown that the thermal conductivity was reduced with increasing CSP
content, which represents a promising diminution of 51% for the incorporation of 30 wt.% CSP.

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This reduction is influenced by the increase in porosity. From the results presented in Fig. 8-d, it

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has been shown that the addition of CSP, which burns during the firing process, leads to an increase
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in the porosity of bricks and thus a decrease in thermal conductivity. However, this reduction in
thermal conductivity is a promising avenue for specific applications, such as thermal insulation,
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which allows for greater energy savings in residential applications [29,30,49].

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Fig. 9. Thermal conductivity of brick specimens (0, 10, 20 and 30% of CSP) sintered at 1100 °C

3.2.5. Microstructural observation (SEM) of clay brick samples

SEM micrographs of the different brick mixtures fired between 900 and 1100 °C are shown in Fig.
10. It is well displayed that the addition of CSP affects the microstructure of the bricks. The images
show an increase in the porosity of the samples as well as the pore size with increasing CSP
addition. Bricks with 30 wt.% CSP incorporation have a large porous texture compared to bricks
with 0 wt.% CSP incorporation. This is related to the combustion of the organic matter present in
the CSP, which releases CO2 and creates a set of pores in the brick bodies. Furthermore, it is also
well shown that increasing the firing temperature improves the densification of the bricks. At 900
and 1000 °C, SEM images illustrate typical heterogeneous microstructures with a wide distribution

29
of pores in the samples. However, the porosity decreases significantly after firing at 1100 °C. The
bodies exhibit a more densified microstructure, which is due to the progressive formation of
anorthite and mullite, which are strong phases contributing to the formation of glassy phases, as
confirmed by X-ray diffraction analysis (Fig.7). An increase in pore size from a spherical shape of
2-5 µm in diameter to an irregular shape up to 25 µm in diameter, according to the SEM scale, is
obtained between 0 and 30 wt.% CSP, which explains the improvement of the mechanical
properties with the decrease of the open porosity compared to bricks fired at 900 and 1000 °C as
reported by [67]. However, the effect of CSP content and firing temperature on brick properties can
be better understood after SEM observation. These results confirm the results of the technological,

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mechanical and thermal conductivity tests (Fig. 8, Fig. 9).

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Fig. 10. SEM micrographs of different brick specimens sintered at 900, 1000 and 1100 °C.

31
 3.2.6. Comparison with previous works

Table 3 provides a summary of the technological and thermal characteristics of fired clay bricks
mixed with various types of waste as pore-forming agents and the processing temperature ranges
used in some recent studies. In order to better understand the features of using wastes as pore-
forming agents, researchers have varied the firing temperature and waste amount, as indicated in
Table 3. Each work's sintering temperature typically ranges between 900 and 1150 °C. Importantly,
the principal crystalline phases (i.e., gehlenite, anorthite, diopside, and wollastonite) occur at
temperatures of approximately 1000 °C, which is consistent with the findings of the current study.
Although, lower sintering temperatures reduce energy consumption in the brick industry, all studies

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have found that mechanical strength values are moderate to higher and more significant after

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sintering at 1000 °C and above [8]. In addition, the waste content affects the overall serviceability
characteristics of fired bricks. The content varied differently in each work, but the common goal

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was to develop porous bricks with optimal physico-mechanical and thermal properties. In all
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research, shrinkage values range from medium to high; in our study, the shrinkage value is reported
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as a medium (0.3-3.8 %) and falls within the normal range [69]. Moreover, the values of bulk
density in all studies are noticed between 1.18 and 2.1 g/cm3 and this is almost similar to our results
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(2-1.15 g/cm3). In our study, bricks fired at 900 °C with 30 wt.% of CSP addition showed higher
porosity and water absorption of around 52.8% and 46.8%, respectively. While Muñoz et al. [63]
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found the highest porosity of 33% with the addition of 17.5 wt.% solid paper residue after firing at
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900 °C. Besides, Ahmad et al. [30] pointed out similar average values regardless of the different
firing temperature (i.e. 1000 °C) with a porosity of 63% for 50% addition of charcoal waste.
However, the increase in porosity improves the thermal insulation of the bricks. In our work,
incorporating 30 wt.% of CSP reduces the thermal conductivity to 0.37 W.m-1.K-1, while Muñoz et
al. [63] found 0.41 W.m-1.K-1 with 17.5 wt.% addition of solid paper residue and Aouba et al. [29]
reached 0.34 W.m-1.K-1 with 7 wt.% addition of wheat straw. Concluding that the technological
and thermal properties of fired bricks are significantly influenced by the type, content and size of
the pore-forming agent, as well as by the sintering temperature.

32
 Table 3. Comparative table of our fired bricks with previous works

Firing Firing Water Thermal

Porosity Pore size Bulk density Mechanical
Sample Pore-agent material temperature shrinkage Absorption conductivity Ref
(%) (μm) (g/cm3) strength (MPa)
(°C) (%) (%) (W.m-1.K-1)
4.8-1.2
Fired clay Eggshell waste,
800-1000 °C – ≈ 14.9-22 – 2.1-1.5 11.1-15.6 (compressive – [8]
bricks (0-15 wt%)

f
strength)

oo
8.3-3.1
Tea Waste, (2.5-

r
1.58-1.37 15.1-21 (compressive 0.61-0.32

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10 wt%)
strength)

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5.4-1.1
Fired clay Corrn cob, (2.5-

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1050 °C – – – 1.69-1.18 12.6-19.4 (compressive 0.61-0.38 [16]
bricks 10 wt%)
strength)

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10.8-3.2
Rice Husk, (2.5-
ur 1.63-1.39 16.5-19.7 (compressive 0.58-0.36
10 wt%)
strength)
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6-1
Lightweight Corn cob waste, (0-
900–1100 °C ≈ 1.7-5.1 ≈ 33.8-48 – ≈ 1.9-1.2 ≈ 17-38 (flexural – [24]
clay bricks 15 wt%)
strength)
36.2-18.1
WheatStraw,
3.8-5.2 27.9-43.5 1.85-1.57 15.3-28.6 (compressive 0.49-0.34
(1-7wt%)
Fired clay strength)
920 °C – [29]
bricks 34-24.8
Olive Stone Flour,
5.5-5.8 29.6-40.6 1.79-1.58 15.2-26.3 (compressive 0.49-0.39
(2-8wt%)
strength)

33
 25 – 4
Coal waste,
0.5-1.7 24-63 – 14–35 (compressive 0.49-0.25
(5-50 wt%)
Fired clay strength)
1000 °C 70–100 [30]
bricks 24.9 – 3
Wheat husk waste,
0.6-1.8 26-65 – 16–37 (compressive 0.35-0.08
(5-50 wt%)
strength)
20.76-10.75
Lightweight Coffee waste, [49]
1150 °C – 17.4-42.8 100-1000 1.66-1.46 13.5-29.25 (flexural 0.73-0.39

f
ceramics (0-30 wt%)

oo
strength)
11-3

r
Fired clay Solid paper residue,

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900 °C 4.3-7.6 ≈ 27-33 – 1.76-1.39 16-24 (compressive 0.53-0.41 [63]
bricks (2.5-17.5 wt%)

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strength)
Coconut shell

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Fired clay 19.46-4.51 This
powder, 900–1100 °C 0.3-3.8 11.9-52.8 5-50 2-1.15 11.21-46.80 0.56-0.37 work
bricks (tensile strength)

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(0-30 wt%)
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34
4. Conclusion
This study evaluated the feasibility of using coconut shells waste powder (CSP) as a renewable
pore-forming agent in fired clay brick making. The effect of coconut shell powder addition and the
variation in firing temperature were investigated. Based on the obtained results, the addition of CSP
did not change the mineralogy and color of the bricks. On the other hand, it appears that the bulk
density decreased with increasing CSP addition, which ultimately leads to lighter bricks. This is due
to pores forming in the brick samples due to the almost complete combustion of CSP. However, the
incorporation of CSP is limited due to the increase in water absorption and the decrease in
mechanical properties. In particular, the combination of firing at 1100 °C with 30 wt.% addition of

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CSP results in clay brick with lower thermal conductivity (0.37 W.m-1.K-1), while maintaining
adequate tensile strength (9.88 MPa). Therefore, the use of CSP as pore-forming agent is a valuable

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way to develop lightweight bricks with promoting thermal insulating character.

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Acknowledgements
This work was financially supported by the National Center for Scientific and Technical Research
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(CNRST), Rabat, Morocco). We thank also the Hassan 2 University, Morocco, through the
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platform of analysis for characterization techniques support.

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Highlights

- Recycling coconut shell waste as a renewable pore-forming agent in fired clay bricks.
- Effect of coconut shell waste content and firing temperature were assessed.
- Technological, mechanical, and thermal behavior of bricks were investigated.

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 CRediT authorship contribution statement

Zineb Moujoud: Investigation, Methodology, Validation, Writing – original draft, review &

editing.

Achraf Harrati: Investigation, Validation, Formal analysis, Writing – original draft, review&

editing.

Ahmed Manni: Formal analysis, Writing – review& editing.

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Amine Naim: Formal analysis, Writing – review& editing.

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Abdeslam El Bouari: Supervision, Validation.
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Omar Tanane: Writing – review & editing, Supervision, Validation.
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Declaration of interests

☒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.

☐The authors declare the following financial interests/personal relationships which may be
considered as potential competing interests:

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