Study of Fired
Study of Fired
Study of Fired
A R T I C L E I N F O A B S T R A C T
Keywords: In the present work, coconut shell powder (CSP) is explored as a pore-forming agent in the
Fired clay bricks manufacturing of fired clay bricks. The bricks were produced by varying the amount of CSP (0,
Coconut shell waste 10, 20, and 30 wt%), and fired at different temperatures (900, 1000, and 1100 ◦ C). Mineralogical,
Pore-forming agent physical, mechanical, and thermal conductivity tests were performed to evaluate the properties of
Thermal conductivity the elaborated bricks. It is found that the addition of CSP does not influence the mineralogy of the
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.K)), 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.
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 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 limited thermal conductivity value, usually about 1.0 ± 0.4 W/(m.K) depending
on the raw materials and the firing process, which means a significant heat loss through the house walls [10]. However, this unfa
vorable property can be solved by introducing pores into the bricks. When pores are created, the thermal conductivity and density of
the bricks are reduced [10–12]. This can be achieved by introducing holes extending through the brick as in the case of a perforated
* Corresponding author.
E-mail address: [email protected] (Z. Moujoud).
https://doi.org/10.1016/j.jobe.2023.106107
Received 28 November 2022; Received in revised form 12 February 2023; Accepted 12 February 2023
Available online 13 February 2023
2352-7102/© 2023 Elsevier Ltd. All rights reserved.
Z. Moujoud et al. Journal of Building Engineering 68 (2023) 106107
brick or by incorporating particles as pore-forming agents in the clay mixture [13,14]. The latter method is widely used by the bricks
industry [14]. When a pore-forming agent is used, the organic matter 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
physico-chemical characteristics, its availability, and its ability to combust completely [14]. 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] 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.K)) compared to OSF (~0.39 W/(m.K)) 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 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. The coconut tree, a member of the
palm tree family (Arecaceae), is grown in more than 100 countries. The global production of coconut is about 250–300 million tons for
the year 2018 [31]. 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 processors as abundant agro-industrial waste or open burned,
creating serious problems in the local 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]. In addition, the use of coconut
shell waste in the building sector has been investigated. Gunasekaran 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.
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.
2.2. Methods
The methodological approach adopted in this study can be resumed as follow: the first step consists of preparation and charac
terization of the raw material (i.e., XRF, CHNS–O, XRD, IR and 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
obtained results present the average of three values.
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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. X-
ray diffraction (XRD) of the raw and elaborated materials was carried out using a BRUKER D8 ADVANCE diffractometer. XRD ex
periments 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.
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.
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
( / ) Mdry ( / )
Bulk density g cm3 = × water density g cm3 (4)
Mwet − Msuspended
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.
The mechanical properties of the fired samples were assessed using an indirect tensile test. The Brazilian Test (diametral
compression) was used to measure the tensile strength of the specimens (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 σ r (MPa) is
given by the following equation [47]:
2×P
σr (MPa) = (6)
π×D×t
where P is the maximum applied load (N), D is the diameter (mm), and t is the thickness of the sample (mm).
Thermal conductivity of brick samples was performed according to the standard ASTM C177 [48] 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-4000 M scanning electron microscope at
an accelerating voltage of 10 kV and using a secondary electron detector (SE).
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Table 1
XRF analysis of red clay and CSP after combustion (Ash state).
Oxide content (wt%) SiO2 Al2O3 Fe2O3 CaO MgO K2O Na2O P2O5 TiO2 LOIa
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 –
a
Loss on ignition obtained after calcination at 1000 ◦ C for 1 h
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Table 2
CHNS–O analysis of the coconut shell powder (CSP) in the raw state.
C 48.4
H 6.8
N 0.13
O 44.59
Cl 0.07
S <0.01
Fig. 1. Particle size distribution of (a) Red clay, (b) Coconut shell powder.
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Fig. 2. XRD diffractograms of raw materials: (a) Red clay and (b) Coconut shell powder.
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. 3. FTIR spectrum of raw materials: (a) Red clay and (b) Coconut shell powder.
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 ◦ C, and their abundances were noticed at 1100 ◦ C.
Gehlenite is formed by a reaction between calcium 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 ◦ C and
completely disappeared at 1000 ◦ C. 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 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 SiO2 at high temperatures; CaO was probably supplied from
calcite and dolomite, however, MgO seems to be originated from chlorite and dolomite; its formation was marked mainly by a sharp
decrease in quartz content [60]. Furthermore, based on the XRD patterns (Fig. 7), the addition of CSP does not modify the mineral
ogical composition compared to bricks without additives, which is confirmed by the appearance of the same formed phases at all
mixtures and sintering temperatures [62].
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Fig. 4. DTA/TG diagrams of raw materials (a) Red clay and (b) Coconut shell powder.
Fig. 5. The morphological aspect of raw materials: (a) and (b) Red clay powder; (c) and (d) Coconut shell powder.
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Fig. 7. XRD diagrams of different bricks fired at (a) 900 ◦ C, (b) 1000 ◦ C, and (c) 1100 ◦ C.
required by the ASTM C62 standard [72]. Therefore, according to ASTM C62 [72] standard, the bricks containing 20 wt% and 30 wt%
CSP can be used for negligible weathering conditions. These bricks may be evaluated in insulation applications where there is no
contact with water. Similar findings have been reported by many researchers [12,73,74].
Fig. 8-f reveals that the tensile strength values are significantly degraded when the additive in the 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 tem
perature. 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,
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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) Apparent porosity
(%), (d) Bulk density (g/cm3), (e) Water absorption (%), and (f) Tensile strength (MPa).
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. 9. Thermal conductivity of brick specimens (0, 10, 20, and 30 wt% of CSP) sintered at 1100 ◦ C.
Fig. 10. SEM micrographs of different brick specimens sintered at 900, 1000, and 1100 ◦ C.
current study. Although, lower sintering temperatures reduce energy consumption in the brick industry, all studies have found that
mechanical strength values are moderate to higher and more significant after 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 was to develop porous bricks with optimal physico-mechanical and thermal properties. In all research, shrinkage values range
from medium to high; in our study, the shrinkage value is reported as a medium (0.3–3.8%) and falls within the normal range [69].
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Table 3
Comparative table of our fired bricks with previous works.
Sample Pore-agent material Firing Firing Porosity Pore size Bulk density Water Mechanical strength Thermal conductivity Ref
temperature (◦ C) shrinkage (%) (%) (μm) (g/cm3) Absorption (%) (MPa) (W/(m.K))
Fired clay bricks Eggshell waste, (0–15 800–1000 ◦ C – ≈14.9-22 – 2.1–1.5 11.1–15.6 4.8–1.2(compressive – [8]
wt%) strength)
Fired clay bricks Tea Waste, (2.5-10 wt 1050 ◦ C – – – 1.58–1.37 15.1–21 8.3–3.1(compressive 0.61–0.32 [16]
%) strength)
Corrn cob, (2.5-10 wt 1.69–1.18 12.6–19.4 5.4–1.1 (compressive 0.61–0.38
%) strength)
Rice Husk, (2.5-10 wt 1.63–1.39 16.5–19.7 10.8–3.2 (compressive 0.58–0.36
%) strength)
Lightweight clay Corn cob waste, (0–15 900–1100 ◦ C ≈1.7–5.1 ≈33.8-48 – ≈1.9–1.2 ≈17-38 6-1 (flexural strength) – [24]
bricks wt%)
13
Fired clay bricks WheatStraw, (1-7 wt%) 920 ◦ C 3.8–5.2 27.9–43.5 – 1.85–1.57 15.3–28.6 36.2–18.1 0.49–0.34 [29]
(compressive
strength)
Olive Stone Flour, (2-8 5.5–5.8 29.6–40.6 1.79–1.58 15.2–26.3 34–24.8 (compressive 0.49–0.39
wt%) strength)
Fired clay bricks Coal waste, (5–50 wt%) 1000 ◦ C 0.5–1.7 24–63 70–100 – 14–35 25–4 (compressive 0.49–0.25 [30]
strength)
Wheat husk waste, 0.6–1.8 26–65 – 16–37 24.9–3 (compressive 0.35–0.08
(5–50 wt%) strength)
Lightweight Coffee waste, (0–30 wt 1150 C
◦
– 17.4–42.8 100–1000 1.66–1.46 13.5–29.25 20.76–10.75 (flexural 0.73–0.39 [49]
ceramics %) strength)
Fired clay bricks Solid paper residue, 900 ◦ C 4.3–7.6 ≈27-33 – 1.76–1.39 16–24 11-3 (compressive 0.53–0.41 [63]
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
(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] found the highest porosity of 33% with the addition of 17.5 wt% solid
paper residue after firing at 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 wt% 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.K),
while Muñoz et al. [63] found 0.41 W/(m.K) with 17.5 wt% addition of solid paper residue and Aouba et al. [29] reached 0.34 W/(m.
K) 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.
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 CSP
results in clay brick with lower thermal conductivity (0.37 W/(m.K)), while maintaining adequate tensile strength (9.88 MPa).
Therefore, the use of CSP as pore-forming agent is a valuable way to develop lightweight bricks with promoting thermal insulating
character.
Data availability
Acknowledgements
This work was financially supported by the National Center for Scientific and Technical Research (CNRST), Rabat, Morocco). We
thank also the Hassan II University, Morocco, through the platform of analysis for characterization techniques support.
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