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PII: S2352-7102(16)30171-1
DOI: http://dx.doi.org/10.1016/j.jobe.2017.03.008
Reference: JOBE234
To appear in: Journal of Building Engineering
Received date: 2 September 2016
Revised date: 11 February 2017
Accepted date: 15 March 2017
Cite this article as: Dsir Tsozu, Aubin Nzeukou Nzeugang, Jacques Richard
Mache, Suilabayuy Loweh and Nathalie Fagel, Mineralogical, physico-chemical
and technological characterization of clays from Maroua (Far-North, Cameroon)
for use in ceramic bricks production, Journal of Building Engineering,
http://dx.doi.org/10.1016/j.jobe.2017.03.008
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Mineralogical, physico-chemical and technological characterization of clays
from Maroua (Far-North, Cameroon) for use in ceramic bricks production
Dsir Tsozua*, Aubin Nzeukou Nzeugangb, Jacques Richard Macheb, Suilabayuy Lowehb,
Nathalie Fagelc
a
Department of Earth Sciences, University of Maroua, P.O. Box 814 Maroua, Cameroon
b
Local Materials Promotion Authority (MIPROMALO), P.O. Box, 2396 Yaound, Cameroun
c
Laboratory of Clays, Geochemistry and sedimentary Environments (AGEs), Boulevard du
Rectorat,17 (Bt. B18) Sart Tilman - 4000, Liege, Belgium
*
tsozudsir@yahoo.fr
Abstract
climate in Far North Cameroon and evaluated their use in ceramic bricks production. Three
samples (Ma1, Ma2 and Ma3) were characterized using XRD, FTIR, XRF and firing at 900,
1000 and 1100C. SiO2 (~64-75%), Al2O3 (~12-15%), Fe2O3 (~2-5%) and (~7%) of fluxing
agents (K2O, CaO, Na2O) were the predominant oxides with a reduce contents in Ma3. Quartz
(~40%), K-feldspar (~25%) and plagioclase (~14%) were non-clay minerals while clays
minerals were mainly kaolinite (~4-10%), illite (~4-7%) and smectite (~2-7%). Ma1 and Ma2
are similar in terms of mineralogy, particle size distribution and plasticity. Sample M3 is most
sandy (65%) and less plastic (2.3%). After firing Ma1 and Ma2 provided good technological
properties compared to Ma3. At 1000C for example, they displayed a metallic sound, bulk
density of 1.8g/cm3, a linear shrinkage <5%, water absorption of 13% and flexural strength
>5MPa. Mixing Ma3 with other samples (up to 50%) substantially improved the quality of the
1- Introduction
Clays are one of the most abundant constituents of the earths surface [1]. They are raw
materials commonly used in ceramic industries. They contain different constituents formed by
weathering of rocks and sediments. Their varieties of uses and properties depend on their
structure and composition [1-3]. Soil fertility for example is largely determined by the
presence of clay. In addition to its agricultural importance, clay has been used for millennia as
building material (bricks), for pottery, body care (masks and mouthwash), for medical uses
(treatment of diarrhoea and gastric ulcers), geopolymer applications and even for
components and different regions of the world use traditional handicraft red clay bricks
which are made of local resources available in the surrounding area [8]. Technological
requirements are often based on the particle size, chemical composition, mineralogical
composition and moisture content [1, 9]. In Cameroon, clay materials occur as residual
product in soil profiles and accumulated materials in some basin or catchment areas [10-12].
Studies carried out in Cameroon belong essentially to the warm and humid tropical zone of
the country [13-15]. In this area, clay materials are characterized by high iron contents whose
influence on mechanical resistance of building materials is well known, and the lack of
fluxing agents as alkali and alkaline earth elements which are necessary for low temperatures
firing. In the semiarid zone of the country on contrary, works on clayey materials are very
rare. In this area, geochemical processes are dominated by bisiallitisation, iron contents are
weak and fluxing agents as alkali and alkaline earth elements are well represented [16, 17]. In
the Maroua region, localized in semiarid zone, alluvial clays are present in all river beds.
They are only exploited for traditional uses, mainly for pottery and traditional bricks. The aim
of the study is to determine the mineralogical, physico-chemical and technological features of
some clay samples found in the Maroua region, and to evaluate their use in the ceramic bricks
production. According to the bioclimatic aspects of local materials like bricks and tiles, these
clayey materials of Maroua can be a solution for housing shortage and thermal comfort in the
The study was conducted in the locality of Maroua, in Far North Cameroon (Fig. 1). The
annual air temperature of about 28.53C. The aridity index (I) of De Martonne [18] shows a
dry season from November to May (I < 20) and a raining season from June to September (I >
20). The rains are concentrated in the two humid months of the year, July and August (I > 50).
The relief of the region is composed of two geomorphological units, hills specifically
inselbergs and plains. The inselbergs are characterized by gentle to steep slopes. They are
formed at the base by a lower to middle Precambrian basement (500 to 600 Ma), mesozonal
to catazonal, composed mainly of gneiss and migmatites [19]. This basement was intruded by
many rocks types of which gabbros are dominant [20]. Plains form the most important unit
dominating the landscape of the whole Far North Region of Cameroon. They are composed
mainly of alluvial deposits of Quaternary age [21]. These plains are drained by many seasonal
stream (or Mayos) with the most important being Mayo Tsanaga, Mayo Mizao and Mayo
deposits were observed in all river banks which enjoy a favourable accessibility, making them
attractive for exploitation in dry season. They were well observed in Mayo Kaliao banks
which were therefore chosen as the study site (Fig.1). Three bulk samples were collected from
three layers of two vertical sections of the Mayo Kaliao banks. The two vertical sections were
distanced by 100 m. One sample was collected in one layer of the left bank and two samples
from two layers of the right bank. The samples were designated Ma1 for the layer of the left
bank, Ma2 and Ma3 respectively for the upper layer and the bottom layer of the right vertical
section (Fig. 2). Samples Ma2 and Ma3 were homogenized and mixed in equal proportion
(50%) to form one mixture called sample "Ma4". The colour observed in the field is gray.
These samples were then characterized in the laboratory in order to highlight the relationships
The particle size distribution was determined by wet sieving for the 80 m fraction
and gravity sedimentation for fraction < 80 m. The Atterberg limits (liquid limit-Wl,
plasticity limit-Pl and plasticity index-IP) were obtained by the Casagrand method. These
analyses were done following the ASTM norm, D-422 and D-4318 respectively.
with Bruker S8 Tiger 4kW spectrometer equipment at Local Materials Promotion Authority
Bulk and clay minerals were identified by X-ray diffraction (XRD) carried out on
disoriented powders and on oriented aggregates. They were obtained with a Bruker Advance
range from 2 to 45 with step size of 0.02 and time per step 2s. Identification of mineral
phases was carried out using Eva software. Further tests for detailed identification were air-
drying (24 hours), glycolation (22 hours) and heating (500C for 4 hours). Qualitative and
semi-quantitative estimation (5-10%; [23] were based on peak intensities of XRD patterns
FTIR spectra (Kbr pellets) with a resolution of 4 cm were recorded on a Bruker Alpha-
P spectrometer.
hydraulic press with a compaction pressure of 3.1MPa, and then dried at room temperature for
72 h, oven-dried (105C). The dried samples were fired at 900, 1000 and 1100C for 5 hours
at a heating rate of 5C per minute in a Multimate furnace. The firing temperature adopted at
work are 900, 1000 and 1100C. The raw materials used are common clays from Maroua
generally favourable for fired bricks. Some of these clays are rich in smectite and fusible
chemical elements during firing. Following the environmental aspect relating to the economy
of energy consumption, it is well known that the ideal temperature to fire bricks must be less
than 1000 C. Also, the region of Maroua is a semi-arid area where source of energy like
wood are very scarce. Colours of raw and fired samples were determined using the Munsell
Soil Color Chart. Sound test was done by knocking the fired specimens with a metal rod. The
firing shrinkage 100(Lm-Lf)/Lm were obtained according to the relative variation in the length
of the specimen, where Lm is the length of the mould and Lf is the length of the fired
specimen. The water absorption and bending strength were determined using ASTM norm
C373-72 and C674-77 respectively. Each result obtained is the average value of 04 samples
tested.
4- Results and discussion
Bulk powder diffractograms revealed the predominance of quartz in all the clay
samples (peaks around 4.25 , 3.34 , 2.45 , 2.12 , 1.85 and 1.54 ). Peaks of feldspar
at 3.24 , plagioclase at 3.18 and anatase at 3.51 were also observed (Fig.3A). At 4.47
, there was the peak associated to clay minerals contribution which in oriented samples
showed the presence of kaolinite (7.16 ), illite (9.95 ) and smectite (15.45 ) (Fig. 3B).
The presence of smectite was confirmed by the glycerol solvation test with the shifting of the
001 peak (from 15.45 to 17.40 ). The diffraction peak at 9.95 and 7.16 were not
shifted during glycolation and further confirmed the presence of illite and kaolinite. The 7.16
diffraction peak disappeared after heating at 500 C while the 9.95 peak was still
observable. The increase of the intensity of diffraction peak at 9.95 after thermal treatment
at 500 C was due to the collapse of the smectite diffraction peak at 10 which is an
additional evidence of smectite. On the quantitative point of view, quartz was the most
abundant mineral, with proportion ranging from 37% to 41%, followed by K-feldspar (23-
34%), plagioclase (12-17%), kaolinite (4-10%), illite (4-7%) and smectite (2-7%) (Tab. 1).
XRD patterns of samples Ma1 and Ma2 were superimposable, indicating similar
mineralogical composition. The difference observed with sample Ma3 mainly focussed on the
clays minerals peaks. Indeed, Ma3 showed the lowest percentage of clays minerals (10%)
while Ma1 and Ma2 presented the highest content (22-24%) (Tab. 1).
The FTIR spectra (Fig. 4) confirmed the high contents in quartz and aluminosilicate
minerals shown by the SiO stretching bands between 9001200 cm-1 or 750-800 cm-1, and
the AlO bending at 400-700 cm-1. The characteristic bands of O-H stretching of kaolinite
appeared between 3695 cm-1 (1) and 3619 cm-1(4). A well crystallized kaolinite generally
suggests that the kaolinite presents in the studied clays was disordered or poorly crystallized
along the (a,b) axes [27]. The disordered or poorly crystallized character of the kaolinite
evidenced by the absence of Al-O-H bending bands at 938 cm-1. This suggests stacking faults
along the c- axis. This confirms the sedimentary origin of kaolinite [27, 28]. The band at
3434 cm-1 could be attributed to the OH vibration of hydroxyl alumina in agreement with [29]
(Fig. 4). The intense band at 1630 cm-1 was attributed to the bending vibration of physisorbed
water molecules. As expected from XRD results, Ma1 and Ma2 spectra were superimposable,
confirming once again the similarity between the mineralogical compositions of the two. One
could also mention the presence of bands between 2900 and 2700 cm-1 (stretching vibration of
the C-H bonds of aliphatic compounds) due to the presence of organic matter in samples.
kaolinite, illite, smectite and trace of anatase (Table 1, Fig. 3). However, kaolinite proportion
of clayey materials obtained in this tropical dry climate was low (<10%). This proportion was
less than those of materials frequently studied in the tropical humid climate zone [10, 11, 14,
conditions in the Far North Region of Cameroon (low rainfall, high temperature inducing high
evaporation and low gradient slopes) which considerably limit the external drainage. Also,
iron contents were low and fluxing agents as alkali and alkaline earth elements were well
represented. The combination of these factors leads to the relative concentration of bases and
silica, as shown by chemical analysis (SiO2 >60%, sum of bases ~7%), and creates favourable
conditions for the genesis of the smectite. The SiO2/Al2O3 ratio is >3%, confirming the
Particle size distribution and plasticity are important parameters to evaluate the use of
Particle size analysis showed that clay fraction (< 2m) ranged from 16.5 to 40%
while that of silts (2<>20 m) and sand (20<>2000m) varied respectively from 17 to
34% and 29 to 36% (Tab. 2). Higher content of clay fraction were observed in Ma1 (36%)
and Ma2 (40%). Ma3 was reach in sand fraction (66%) and deficient in clay fraction (16.5%),
in line with a high proportion of quartz fraction observed in XRD analysis. According to
Winklers diagram, sample Ma1 and Ma2 were suitable for thin-walled hollow bricks and
roofing tiles lightweight bricks, and Ma3 was classified for solid brick making (Fig. 5a).
Plasticity of all samples varied between 2.3 25.7% (Tab.2). In the Casagrand's
diagram, the studied alluvial clays belonged to the domain of low plastic clay (Ma3) and illitic
medium plastic clay (Ma1 and Ma2) [31] (Fig. 5c). The high quartz contents constituted the
main factor responsible for lowest plasticity noted in Ma3. The plasticity index (PI) values of
Ma3 lower than 10% implied that this sample is not appropriate for building-related ceramic
production due to the risk of inappropriate extrusion process [32] (Fig. 5b). The plasticity
index values of Ma1 and Ma2 higher than 10% on contrary might be successfully used to
produce structural clay products by extrusion process. The mixture Ma4 was also good for
test the fusibility of clays for ceramic bodies [30,33]. Chemical data of studied clays
correlated with their mineralogical composition. The main oxides for all samples were SiO2
(64-77%), Al2O3, and Fe2O3 (Table 2). Al2O3 contents were not very high (11-15%) and the
proportion of iron oxide Fe2O3 was significant (2-5%). Ma3 was more siliceous (77%) with
less iron (2%). Silica and alumina contents agreed respectively with the quartz and kaolinite
contents. The LOI (13%, 8% and 2%) was low compared with entirely kaolinitic clays (14%)
and also indicated a greater amount of impurities (quartz, feldspar). The sum of
exchangeable bases (K2O, Na2O, MgO, CaO) was high (around 7%), implying that these
studied clays integrated fluxing minerals. The presence of feldspar, illite and smectite could
guarantee a good fusibility of the bricks principally for Ma1 and Ma2 in which illite and
Ma2 were almost similar, but different with those of Ma3 which was sandier in composition.
Samples Ma2 and Ma3 were homogenized and mixed in equal proportion (50%) to form one
mixture called sample "Ma4". The firing properties of bricks specimens show a metallic
sound and very good cohesion for samples Ma1, Ma2 and the mixture Ma4 (at 1100C)
(Table 3). No cracks were observed in all specimens as shown in Fig. 6. This metallic sound
probably reflects the maturity of the fired products [34]. Apart from the resonance, the bulk
density, linear shrinkage, water absorption and the flexural strength were also used to access
The bulk density of the fired products which increased with the firing temperature
varied between 1.7 to 2 g/cm3 and was slightly lower for Ma3 (1.6 g/cm3). The high value of
the bulk density (2 g/cm3) was observed at 1100C, confirming the mineralogical
The linear shrinkage values of the bricks increased with increasing firing temperature
(Tab. 3). At < 1000C, the values were less than 3% (Ma1 and Ma4), 5% (Ma2), and 0.2%
(Ma3). These values rose to 6% (Ma1), 8% (Ma2), 1.2% (Ma3) and 3% (Ma4) when the
temperature reached 1100C. This shrinking and bulk density behaviour, primarily attributed
to the degree of sintering and initial porosity of the green body, is probably due to
rearrangement reactions within the firing product associated to partial sintering of some
phases [35]. Ma3 presented the lowest shrinkage values (0.1 to 1.2%). Ma2 showed a higher
linear shrinkage (4 to 8%), after Ma1 (2 to 6%) and Ma4 (0.8 to 3.1%), suggesting a positive
The water absorption values decrease with increasing firing temperature (Tab. 3).
These values were 13.8% and 12.5% (at 900C), around 13% and 12% at temperature <
1000C and decrease again to 6-7% at 1100C for Ma1 and Ma2 samples respectively. For
Ma3, values were around 17-18% at temperature below 1000C and decreased to 13% at
1100C. The mixture Ma4 portrayed a positive effect by reducing the percentage of water
absorption, which varied with firing temperature (13% from T<1000C) to 10% at 1100C.
Considering the reported value (less than 20%) of water absorption recommended for fired
brick in tropical countries [34], the produced bricks remain acceptable. All the studied bricks
presented an increase of the bending strength from 900C to 1100C. The low values of
bending strength attributed to Ma3 (< 3MPa) were probably due to the poor fusibility of this
sample, correlated to the low content of clayey minerals (illite and smectite). Also, all
samples with high values of water absorption show low values of bending strength. This may
be due to the fact that in the absence of liquid phase, the rearrangement would not lead to a
strong densification. Consequently, the open porosity is high. At temperatures near 1000C,
the bending strength increase from 5 or 6 MPa to 10 MPa (sample Ma1 and Ma2) and from 3
MPa to 6MPa (sample Ma4). The admixture of Ma2 in the Ma3 slightly increased the bending
strength values; this may arise from the ongoing reaction of the fusibility phases brought by
Ma2 sample. At high temperature the increase value may probably be related to phase
transformations like mullite formation [8, 10, 15]. According to [36], 7 MPa is the minimum
value required for normal fired brick. The alluvial clays studied could be used for industrial
production of fired bricks and the minimal firing temperature required is 1000C.
5- Conclusion
The main aim of the present work was to determine the mineralogical, physico-chemical and
technological features of three clay samples found in the Maroua region in dry climate, and to
evaluate their use in the ceramic bricks production. The main results revealed that the clays
deposit in Maroua region consist mainly of clayey portions (Ma1 and Ma2) and sandy
portions (Ma3). Ma3 shows a lower percentage of clays contribution (10%) while Ma1 and
Ma2 present the higher content (22-24%). The mineralogical composition of samples includes
quartz (37-41%), k-feldspar (23-24%), plagioclase (12-17%), kaolinite (4-10%), illite (4-7%),
smectite (2-7%) and trace of anatase (3%). From the physico-chemical properties, the alluvial
clays were classified as medium plastic clays (Ma1 and Ma2) to low plastic clay (Ma3).
According to their firing properties, the studied natural clays are suitable for brick-making
except Ma3, which can be suitable unless after adding fusibility clay like Ma2 to control the
shaping.
Acknowledgments
The authors are grateful Dr Kenne Dedzo Gustave from the University of Yaound 1 for his
contribution. We also thank Dr Cornelius Tsamo for English editing. We are glad for the
comments and suggestions of the anonymous referees who have substantially improved the
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prerequisite for local material promotion, J. Afr. Earth Sci. 55 (2009) 6978.
[15] Ndjigui P-D., Mbey J.A. Nzeukou Nzeugang A., 2016. Mineralogical, physical and
mechanical features of ceramic products of the alluvial clastic clays from the Ngog-
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[17] Nguetnkam, J.P., Villiras, F., Kamga, R., Ekodeck, G.E., Yvon, J., 2014. Mineralogy and
conditions in the extreme North Cameroon (Central Africa). Chemie der Erde 74, 185-
193.
[18] De Martonne, E. (1926). Arisme et Indice dAridit. Comptes Rendus Acadmie des
[19] Kouske, A.P., Suh, C.E., Ghogomu, R.T., Ngako, V., 2012. Na-Metasomatism and
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[20] Lasserre, M., 1975. Etude de Gologique et prospection gnrale oriente du complexe
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[22] Moore Duane M. and Reynolds Robert C. Jr., 1989. X-Ray Diffraction and the
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for building clay products: a reappraisal of the Winkler diagram. Clay Minerals, 33,
435-442
[31] Holtz R.D. and Kovacs W.D. 1981. An introduction to geotechnical engineering.
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Fig 1: Localisation of residual clays in Maroua, Far-North, Cameroon (a). Geological map of
Fig 2: Vertical sections across the alluvial deposits of the Mayo Mizao River banks (A: left
Fig 3: XRD patterns of samples (A): Bulk XRD pattern, K: kaolinite, Q: Quartz; K-Felds:
Feldspar; Pla: Plagioclase. (B): Clay < 2 m pattern. N: air dried condition; EG glycolated
condition with ethylene glycol for 22h; H: heated at condition (500 C for 4 h).
Fig 5: Evaluation of the suitability of raw material base on empirical diagrams. (A) Diagram
of Winkler (1954) in [1], showing suitable mixtures of grains fractions for solid brick (1),
vertically perforated bricks (2); roofing tiles lightweight bricks (3) and thin walled hollow
bricks (4). (B)Diagram of Bain and Highley [32] showing sample good for brick (Ma3),
samples acceptable (Ma1, Ma3) or optimum (mixture Ma4) in extrusion brick-making. (C)
Diagram of Holtz and Kovacs [31] showing the illitic character of Ma1 and Ma2.
Mineralogical
Minerals Measured intensity CF* References Composition %
of reflection d() Ma1 Ma2 Ma3
Powder Quartz (3.34 ) 3.37-3.31 1 37 41 41
K- feldspar (3.24 ) 3.26 3.21 4.30 Cook et al., 1975 25 23 34
Plagioclase(3.18 ) 3.21-3.16 7 12 12 17
Anatase (3.51 ) 3.54 -3.50 3 1 0
Booski et al. 1998 in
Argile (4.47 ) 4.4 20 Fagel et al. 2003 22 24 10
Highlights
Alluvial clayey materials from semi-arid climate in Far North Cameroon were
evaluated for their use in ceramic bricks production.
Their mineralogical composition included quartz, k-feldspar, plagioclase, kaolinite,
illite, smectite and trace of anatase.
The alluvial clays were classified as medium plastic clays to low plastic clay.
After firing medium plastic clays provided good technological properties and
properties of low plastic clays were substantially improved by mixing them with other
samples.
To Mora 141604 To Mora 142134
400
Mount Boulor Kodek
Mambang 860 Gayak
To Guirvidig
Mozogo
Djarengol Kodek
MTchoffabani
MAROUA Kongola
To Yagoua
ay o
Mi
za o
Zaka 722
Kaliao Dougo
Cameroon
Dourga Palar
Maroua
al i ao
oK
M ay
103500 103500
Dakar
Madaka
a
Ngassa
g
na
Miskine
sa
703
oT
y
Ma
Hosr Makaba
141604 To Garoua To Mindif 142134
0 5km
Key
Study site Road
Fig. 1.
Vegetation
Sampling point
Fig. 2.
A
d=3.34 Q
d=3.24
(A) d=4.47 K-felds
Total clay
d= d=1.54
4.25Q d=3.18 Pla d=1.85 d=1.31
d=14.75 S Q Q
d=2.45 d=2.12 Q
d=1.67
d=7.17 K Q Q
Q
MA3
MA2
MA1
0 10 20 30 40 50 60 70
2 CuK1
d=15.45
Smectite d=9.95
d=15.45
Illite
Smectite
500
d=9.95 500 d=15.45
MA3
Illite 500
MA1 d=9.95 MA2 Smectite
Illite
d=7.16
Kaolinite
EG d=7.16
Kaolinite d=7.16
Kaolinite EG
EG
N
N
d=4.99 N d=4.99
d=4.99 Illite/smectite
Illite/smectite Illite/smectite
(B)
2 4 6 8 10 12 14 16 18 20 0 2 4 6 8 10 12 14 16 18 20
0 2 4 6 8 10 12 14 16 18 20
2 CuK1 2 CuK1 2 CuK1
Fig. 3.
1,8
1038
1,6
1,4
468
1,2
533
Ma1
1
Ma2
0,8
914
Absorbance
3434
3620
Ma3
693
3695
0,6
1630
0,4
0,2
-0,2
4000 3500 3000 2500 2000 1500 1000 500 0
Wavenumber cm-1
Fig. 4.
<2m
0 100
20 80
50
45 Ma1 Ma2 Ma3 Ma4
(A) 40
70
Non Low Medium Highly
60 plastic plastic plastic plastic
Illite
50
Plastic index (%)
Montmorillonite
40
Kaolinite
30
Ma1
20 Ma2
Ma3
10
Chlorite Ma4
0
0 20 40 60 80 100
(c) Liquid limit (%)
Fig. 5.
Fig. 6.