i An update to this article is included at the end

Case Studies in Construction Materials 11 (2019) e00262

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Case Studies in Construction Materials

journal homepage: www.elsevier.com/locate/cscm

Case study

Development of unfired earthen building materials using

muscovite rich soils and alkali activators
Emeso Beckley Ojoa,*, Kabiru Mustaphab , Ronaldo S. Teixeirac ,
Holmer Savastano Jrc
a
Department of Materials Science and Engineering, African University of Science and Technology, Nigeria
b
Department of Materials Science and Engineering, Kwara State University, Malete, Nigeria
c
Department of Biosystems Engineering, University of Sao Paulo, Pirassununga, Sao Paulo, Brazil

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

Article history: Most studies have focused on the alkali activation of thermally activated kaolinitic clays for
Received 26 February 2019 the production of innovative building materials. Whilst the widespread use of these
Received in revised form 10 June 2019 minerals may be hindered due to geographical availability; a combination of thermal
Accepted 14 June 2019
activation and alkali activator solutions yields a material with high embodied energy with
implications on eco-friendliness. This study presents an eco-friendly approach for the
Keywords: development of a low environmental impact building material using a low molarity alkali
Unfired earth
activator solution for the stabilisation of uncalcined muscovite rich soil. Influence of curing
Building materials
Muscovite
conditions on the physical, mechanical, microstructural and mineralogical properties were
Compressive strength evaluated. Results show that alkali activation of uncalcined muscovite in the soil
Alkali activators significantly improved the physical and mechanical properties of extruded earthen
materials. Samples tested yielded compressive strength values between 9–11 MPa for
varying curing regimes. The binding was mainly attributed to the formation of amorphous
sodium aluminosilicate gels as a result of the partial dissolution of muscovite. These results
show that low environmental impact building materials may be developed with uncalcined
muscovite rich soils in developing regions around the world where these minerals are
predominant for the provision of sustainable low-cost housing solutions.
© 2019 The Authors. Published by Elsevier Ltd. This is an open access article under the CC
BY-NC-ND license (http://creativecommons.org/licenses/by-nc-nd/4.0/).

1. Introduction

Owing to environmental challenges associated with the production of cement, significant research has focused on alkali
activated materials as alternative binders in construction materials [1,2]. Presently, extensive studies have demonstrated the
improved properties of alkali activated aluminosilicates over conventional Portland cement in concrete [3–5]. However, very
little work has been conducted to harness this technology for the development of earthen construction building materials. In
a practical sense, 65% of the earth crust comprises of natural aluminosilicates and this triggers the interest to determine if
alkali activation can be harnessed for the production of building materials from soils containing these minerals. Such
information will enhance the adoption and commercialisation of a new promising technology for the development of
construction materials. In theory, any material composed of silica and aluminium can be alkali activated. This has been

* Corresponding author.
E-mail addresses: eojo@aust.edu.ng (E.B. Ojo), kabiru.mustapha@kwasu.edu.ng (K. Mustapha), ronaldost@usp.br (R.S. Teixeira), holmersj@usp.br
(H. Savastano).

https://doi.org/10.1016/j.cscm.2019.e00262
2214-5095/© 2019 The Authors. Published by Elsevier Ltd. This is an open access article under the CC BY-NC-ND license (http://creativecommons.org/
licenses/by-nc-nd/4.0/).
2 E.B. Ojo et al. / Case Studies in Construction Materials 11 (2019) e00262

discussed by studies carried out by Xu and van Deventer [6] on the alkali activation of 16 natural aluminosilicate materials.
Their results confirm the reactivity of a wide range of aluminosilicates at varying dissolution rates. However, with the
variable mineralogical composition of soils, it is not possible to know if alkali activation would provide a sufficient
mechanism for the stabilisation of soils.
Prior work by Davidovits [7] proposed the Low Temperature Geopolymeric Setting (LTGS) as a stabilization mechanism
for the production of high mechanical strength and water stable building units at drying temperatures of 50–250
C. The
authors reported that kaolinite mineral in clay/lateritic soils can be transformed into a three dimensional compound
producing water stable building blocks with satisfactory mechanical properties (comparable to fired bricks) using alkali
activators. In related studies, Slaty et al. [8] demonstrated alkali activation of kaolinitic clays using NaOH with mass ratios of
8–20% in the production of composites with satisfactory mechanical properties both in the dry and saturated condition.
However, results from Maskell et al. [9] demonstrated that this mechanism was ineffective for the stabilisation of a
predominantly silty soil containing kaolinite using varying NaOH contents. Phase composition of these aluminosilicate
precursors has been identified as a critical variable which determines the reactivity and thus the degree of dissolution [10] in
alkaline environment. This has necessitated the de-hydroxylation of clay minerals to break down the crystalline structure in
order to increase reactivity. However, de-hydroxylation would entail heating to temperatures above 500
C with attendant
effect on embodied energy of the building material. Alternatively, high concentration alkali activation solutions may improve
dissolution rates as the quantity of alkaline activator added to the argillaceous material determines the level of crosslinking
resulting in the formation of water stable units Davidovits [7,11]. However, the addition of high alkaline concentrations may
negate the environmental benefits of unfired earth as a sustainable construction material. According to Maskell [12], the
inclusion of chemical additives to unfired earth has a detrimental effect on embodied energies and global warming
potentials. The production of alkali activators constitutes the most energy intensive component of the production process
[13] and hence, a smaller energy footprint may be obtained by promoting the use of low molarity solutions. Furthermore, the
use of high alkaline sodium hydroxide solutions may not be practical for large scale production processes.
Relative to kaolinite minerals, published results on the products of alkali activation of muscovite minerals are scarce.
Muscovite rich soils are predominantly located in large reserves in United States, Africa and South America as well as India
and China [14]. Muscovite mineral is a 2:1 dioctahedral phylosilicate predominantly found in sedimentary and metamorphic
rocks [15] and is one of the main rock forming minerals found in granites, pegmatites and schists. Given their abundance,
they have the potential to serve as alternatives to kaolinite minerals in these regions for the provision of low-cost housing
solutions. Pacheco-torgal et al. [16–18] demonstrated the possibility of using a tungsten mine waste containing muscovite
and quartz for the production of alkali activated binders. However, the starting material was dehydroxylated and may
present different reactivity levels relative to the uncalcined material. This current research contributes to this field by
presenting results on the application of alkali activation of muscovite rich soils for building construction purposes.
The objective of this study was to explore the role of alkali activation as a viable stabilisation mechanism for production of
earthen building units from muscovite rich soils. The production of alkali activators constitutes the most energy intensive
component in the use of alkali activated binders. Hence, the focus of the study was to develop low-impact building material
using lower bound molarity concentrations reported in literature as constants but initial curing temperature as variables.
With increasing demands for kaolinite as source materials for various industrial processes, the feasibility of using other
prevalent clay minerals (such as muscovite) is evaluated in this study. The experimental methodology involved
characterising the soil to identify the mineralogical composition, producing specimens using the extrusion technique,
evaluating the mechanical and physical properties as well as microstructural/mineralogical characterization. Commerci-
alisation of alkali activation technology is advancing in various parts of the world and the implication of this study may
provide a low embodied energy approach of harnessing alkali activation technology in the production of unfired earthen
building materials.

2. Materials and methods

2.1. Soil

The soil used for this study was supplied by Top Telha Ceramic Tile Company, Leme and sourced from Brazilian quarries in
the State of Sao Paulo, Brazil. The soils are typical source materials used for the production of fired clay roof tiles. The grain
size distribution of the soil was determined by mechanical sieving and hydrometer sedimentation in accordance with BS
1377:2 and showed 68% of particles finer than 75 mm. In accordance with BS1377:2, atterberg limits for the soil were 42.5%
and 20.0% for liquid limit and plastic limit respectively (Table 1). Based on the unified soil classification system (USCS), the
soil was classified as CL (inorganic clays of low plasticity). These properties do not fit the criteria required for ideal soils for
cement stabilisation; suitable soils should be generally coarse grained soils with low clay fractions and plasticity index of 5–
15%. Soils with higher plasticity values are characterised by low compressive strengths, inadequate durability and excessive
drying shrinkage [19].
Characterization was carried out by Scanning Electron Microscopy with chemical analysis by Energy Dispersive X-ray
Spectroscopy (EDX). Fig. 1 shows the Back Scatter Electron image of the as-received samples showing wide variation of
particle sizes. Particles are predominantly irregular shaped and with smaller sized particles agglomerating over larger
particles. Particles range in diameter from as high as 0.4 mm to a few micrometers. The elemental composition of the soil
 E.B. Ojo et al. / Case Studies in Construction Materials 11 (2019) e00262 3

Table 1
Properties of soil.

Characteristics %
Atterberg Limits
Liquid Limit 42.5
Plastic Limit 24.9
Linear Shrinkage 9.18
Particle Size Distribution
Sand 35
Silt 33
Clay 32
Mineral Content
Muscovite 52.5
Quartz 32.7
Sanidine 12.9
Chemical Composition
SiO2 70.39
Al2O3 13.31
Fe2O3 4.09
K2O 4.97

expressed in oxides show silica and alumina as the major components of the soil at 70.4% and 13.3% respectively. Other
predominant elemental oxides are reported in Table 1. X-Ray Diffraction (XRD) was performed using a Rigaku MiniFlex 600
with range 10-70
(2u) at a rate of 0.02
/min and showed mineralogical composition to be predominantly muscovite, with
traces of quartz and sanidine (Fig. 2).

2.2. Alkali activators

Sodium hydroxide used was of caustic soda pellets with 97% purity whilst sodium silicate was in powder form. Both
activators were supplied by Dinamica Quimica Contemporanea Ltd, Brazil. The chemical composition of sodium silicate
powder comprised 18% Na2O and 63% SiO2. The alkali activators; sodium hydroxide and sodium silicate were applied in the
proportion of 3.0% and 0.75% respectively, in relation to the soil mass. Studies by Davidovits [11] showed that the minimum
sodium hydroxide content required to achieve water stable units was 3% NaOH content by dry weight of soil. As a result, this
minimum stabilisation content was adopted to ensure that the building units had minimal environmental impact. In
addition, sodium silicate was included in the activator solution as it is commonly used to hasten the reaction by providing
readily available Si in the reaction. Different studies have shown that a sodium hydroxide to sodium silicate ratio of 0.22–0.25
yields optimum results [20]. As a result, a mass ratio of 0.25 was adopted in this study.

2.3. Production of samples

The method of production of specimens adopted in this study was largely based on studies conducted by Maskell et al.
[9,21,22] on production of unfired extruded earth bricks. This method of production closely represents the industrial
production of extruded fired bricks (without the kiln firing process) to allow for easy adoption of innovative processes in

Fig. 1. Backscatter Electron Images of clay.

4 E.B. Ojo et al. / Case Studies in Construction Materials 11 (2019) e00262

Fig. 2. XRD spectra of clay.

already existing factories. These studies have shown that the optimum moisture for extrusion moulding is typically within
the range of the plastic limit of the soil as extrusion at moisture contents lower than the plastic limit result in notable surface
cracking [23]. Hence, a moisture content corresponding to the plastic limit of the soil (25%) was adopted.
In the preparation sequence, sodium hydroxide pellets and sodium silicate powder were dissolved into the required
amount of water and the solution allowed to cool for 24 h given the exothermic nature of the dissolution. The mixture was
homogenised in a high energy intensive Eirich mixer (capacity 10 L) for 5 min at high speed and transferred to a Gelenski
MVIG-05 laboratory extruder operating at a linear speed of approximately 4 mm/s. Cylindrical samples were extruded with
diameter 40 mm and height of 80 mm for axial compression tests. The curing regime was varied to ascertain if alkali
activation process would be accelerated through an initial elevated curing temperature as well as additional curing at room
temperature. A minimum of six specimens were cured in the laboratory environment at a room temperature of (24  3)
C
and 60% RH for duration of 7 and 15 days. Another set of specimens were cured initially at elevated temperatures (60 and
105
C) for 5 h and left in the laboratory at room temperature (24  3)
C and 60% RH and tested after 7 and 15 days. Studies
have shown that optimum curing temperature is a function of NaOH concentration with lower optimum curing temperature
corresponding to low NaOH concentration [24].

2.4. Experimental program

2.4.1. Stability in water

The water sensitivity test was conducted to serve as an indicator of the viability of this mechanism for the stabilisation of
clay minerals particularly at low alkali concentrations. The water stability was assessed by full immersion of samples after 15
days in deionised water at room temperature (24  3)
C for 24 h. Treated and untreated samples subjected to the various
curing conditions were also immersed in water for 24 h and evaluated by physical assessment.

2.4.2. Physical characterization

Physical characterization comprised evaluation of water absorption, bulk density and apparent void volume according to
BS EN 772-4:1998. A minimum of five specimens each were subjected to physical tests. Physical properties were obtained
using Eqs. (1)–(3):
 
Msat  Mdry
Average Void Volume ð%Þ ¼  100 ð1Þ
Msat  Mi

 

Mdry
Bulk Density  g=cm3 ¼   r ð2Þ
Msat  Mi

 
Msat  Mdry
Water Absorption ð%Þ ¼  100 ð3Þ
Mdry

where Msat is the saturated specimen’s mass with a dry surface, Mdry is the dry specimen’s mass after 24 h at 105
C, Mi is the
specimen’s mass immersed in water and r is the bulk density of water (g/cm3).
 E.B. Ojo et al. / Case Studies in Construction Materials 11 (2019) e00262 5

2.4.3. Mechanical characterization

Mechanical characterization entailed evaluation of strength under axial compression using a Universal Testing Machine
(Emic DL-30000 model) equipped with a 1 kN load cell. There is presently no consensus on the appropriate procedure for the
evaluation of unconfined compressive strength of unfired earth [25]. Testing procedures are often based on those used for
concrete or fired bricks. Unconfined compressive strength was evaluated using procedure adopted in Maskell et al. [22]
which is a modification of BS EN 772-1:2000. The study showed there was no significant variation associated with capping
small scale specimens. Hence, tests were conducted on uncapped specimens which were sufficiently flat. According to
Walker [26], moisture content at testing plays a significant influence on mechanical strength and it’s important to
standardize moisture contents before testing. As a result, mechanical properties of the test pieces were evaluated under two
pre-conditions: oven-dry condition (60
C for 24 h) and fully saturated condition (total immersion in water for 24 h).

2.4.4. Statistical analysis of mechanical properties

To aid in the interpretation of results, statistical analysis was performed using ANOVA analysis in order to ascertain effect
of curing conditions on the mechanical properties. One-way ANOVA tests were used to determine if differences existed
between population means obtained at varying initial curing temperatures. The procedure tested the null hypothesis (Ho)
that the average results for all curing conditions are equal (suggesting that the initial curing temperature had no effect on the
compressive strength) against the alternative hypothesis (Ha) that at least one average result was different i.e
H0 : m1 ¼ m2 ¼ m3
ð4Þ
Ha : At least  one  mean is dif f erent f rom the others
where m1, m2, and m3 are population means corresponding to different curing conditions. A significance level of 5% was
adopted for this study indicating that if the p-value of a statistical test was less than 0.05, at least one of the population
means was statistically different from the others and the null hypothesis (Ho) was rejected. If Ho was rejected, a post-hoc test
(Tukey’s Honestly Significance Difference (HSD) test) was performed to determine which means were statistically different
from each other.

2.4.5. Scanning Electron microscope (SEM) and EDX analysis

Scanning electron microscopy (SEM) was used with a Back-Scattering Electron (BSE) image detector, operated at 15 kV
accelerating voltage, for visualization of the surface of the microstructure using a Hitachi Tabletop Microscope TM3000 with
a coupled X-ray energy dispersive spectroscopy system. Sample preparation was accomplished with impregnation using
epoxy resin. The samples were manually polished in a Struers TegraPol-11 machine using silicon carbide abrasive paper
using grit sizes 320, 600, 1000 for 6 min, with alcohol as lubricant. Samples were polished using 6, 3, 1 mm diamond
polishing compound for 6 min.

2.4.6. X-Ray diffraction

X-Ray Diffraction (XRD) was performed using a Rigaku MiniFlex 600 with range 10-70
(2u) at a rate of 0.02
/min and Cu
Kα to identify crystalline phases in materials. XRD spectra of samples cured at varying temperatures and tested after 15 days
were analysed and compared with the starting material in order to detect any significant modification in its mineralogical
structure.

2.4.7. FTIR spectra analysis

FTIR spectra were acquired using a Thermoscientific Nicolet IS5 spectrophotometer operating in absorbance mode. The IR
spectra were acquired between 400 and 4000 cm1 (resolution of 4cm-1). Each sample was pulverised and mixed with dry
KBr powder prior to analysis. FTIR spectra of treated samples was analysed to characterise modifications in molecular
bonding in order to ascertain degree of modification of starting minerals.

3. Results and discussion

3.1. Effect of initial curing temperature on stability in water

Typically, unstabilised earth tends to disintegrate upon direct contact with water, limiting its use to internal controlled
walling systems. This limitation has been attributed to the presence of clay minerals in the soil. As a result, studies have
shown that a good indication of durability of earthen materials for construction is an assessment of its stability in water
[19,26]. According to Davidovits [11], bricks produced from the geopolymerisation of kaolinitic clays produced a 3-D
structure that was water stable. Although authors have argued that testing in the saturated condition is considered
inappropriate for unstabilised earth [27], as application of this class of materials should be restricted to moisture-controlled
environments; an attempt was made to evaluate under this condition to ascertain the degree of stabilisation obtained
through alkali activation with low molarity solutions. Achieving water stable units would also indicate that the application of
unfired earth may subsequently be expanded to uncontrolled moisture exposure conditions or extreme weather events such
as flooding. Fig. 3 presents moisture resistance of alkali activated specimens tested after 15 days.
6 E.B. Ojo et al. / Case Studies in Construction Materials 11 (2019) e00262

Fig. 3. Behaviour in water of samples cured at different initial curing temperatures: (a) room temperature (b) 60
C and (c) 105
C.

As observed in Fig. 3, samples cured at room temperature and initial curing temperature of 60
C showed high sensitivity
to water. Failure of samples cured at room temperature was characterised by a complete delamination of outer surface
followed by disintegration of samples into soil lumps (Fig. 3a). Total disintegration would suggest an absence of binder
whereas disintegration into lumps, as observed with these samples, suggests that some reaction took place particularly at
the surfaces of the samples but was insufficient to produce sufficient binding to withstand internal pore pressures
development during water immersion. Also, samples cured at 60
C disintegrated initially by the formation of multiple crack
patterns on the surface (Fig. 3b) prior to partial disintegration into soil lumps. This behaviour is contrary to results obtained
from the alkali activation of kaolinitic minerals where curing at room temperatures produced sufficient binding to attain
water stable units even at low alkaline solutions [11]. However, as observed in Fig. 3c, only samples cured at 105
C were
stable in water. This indirect method of ascertaining extent of stabilisation with low alkali concentrations suggests that,
unlike kaolinitic soils, muscovite rich soils require elevated curing temperatures to attain sufficient stability in water.

3.2. Physical characterisation: water absorption, density and apparent porosity

Water absorption, density and apparent porosity were determined using the water displacement method. Since samples
cured at room temperature and 60
C were not water stable, only samples cured at 105
C could be tested. Results from the
physical tests reveal an average water absorption of 22% with standard deviation of 0.63%. This absorption capacity gives an
indication of the presence and significance of voids [28]. Similar high water absorptions have been reported in cement
stabilisation of fine grained soils [29] and this has been related to clay content. These values may be attributed to the
predominantly fine-grained nature of the soil, which resulted in increased soil suction as a result of smaller pore spaces. Seco
 E.B. Ojo et al. / Case Studies in Construction Materials 11 (2019) e00262 7

et al. [30] correlated water absorption behaviour of stabilised earth blocks to outdoor exposure over time and reported water
absorption to be a satisfactory indicator of durability of earth blocks. The average void volume of 36.6% (with standard
deviation of 0.79%) recorded suggests that about one-third of the samples comprises of voids. These values are indicative of a
low packing density and poor contact among particles. This could be attributed to the soil grading as well as production
method adopted. Studies have shown that manufacturing process determine mechanical performances of unfired earth [31].
It is possible that a lower moulding moisture content (for instance, the optimum moisture content) of the soil would have
resulted in an improved packing density. Given the linear relationship between porosity and strength of unfired earth [29], it
is expected that extrusion of samples on the dry side of the plastic limit may yield samples with improved mechanical
properties. However, it is important to note that high porosities in earthen construction induces low thermal conductivities
in the building units [32] which is significant in passive design of buildings. An average bulk density of 1.66 g/cm3 (with
standard deviation of 0.013 g/cm3) was recorded; this falls within the lower bound of values typically obtained for earthen
building materials. This low density presents useful applications as lightweight construction materials.

3.3. Mechanical characterisation: compressive strength

Fig. 4 presents test configuration and typical failure mode observed with the specimens. Failure was characterized by the
formation of near vertical surface cracks and exfoliation of the lateral sides in all cases. This would indicate the compressive
stresses resulted in inelastic deformations to the specimens causing the lateral sides to exfoliate and fall off. The samples
demonstrated some considerable cracking and deformation before failure. Despite the loss of the sides, the central core
remained intact after testing.

3.4. Effect of initial curing temperature on compressive strength

In this study, effect of initial curing temperature (I.C.T) on the alkali activation of muscovite rich soils was evaluated by
subjecting the samples to three different I.C.T (room temperature, 60
C and 105
C) for 5 h. Following initial curing, all
samples were subjected to additional room temperature curing and tested after seven days and fifteen days. Fig. 5 presents
variation of compressive strength with initial curing temperature for samples tested in oven-dry and saturated conditions.
After 7 days curing at room temperature, samples tested in the oven-dry condition yielded an average peak stress of 9 MPa;
whilst initial curing at elevated temperatures (60
C and 105
C) for 5 h, resulted in average compressive strength of about
10 MPa and 11 MPa respectively (Fig. 5a). These values clearly exceed minimum strength requirements of 2.9 MPa defined for
stabilised earthen walling units tested in the dry condition as reported in Maskell et al. [23].
Results from the ANOVA analysis reveal that only compressive strength obtained from samples cured at I.C.T of 105
C was
statistically different from strengths obtained at 60
C and room temperature at this age. This would suggest that only initial
curing at 105
C significantly influenced the alkali activation process. This could explain results obtained from water stability
assessment. Again, this behaviour deviates from results from alkali activated kaolinitic minerals where curing temperatures
below 60
C significantly influenced alkali activation process (8). Nonetheless, results obtained in this study are comparable
to values obtained in alkali activation of other clay minerals; Slaty et al. [8] obtained compressive strength of 12 MPa at 8%
NaOH addition to kaolinitic soils whilst at 3% NaOH content, Davidovits [11] obtained 15 MPa after curing at 85
C. These
results demonstrate potential of alkali activation as a suitable binding mechanism for muscovite rich soils. On the other
hand, much lower values have been reported in cement stabilised earth blocks. Ojo et al. [33] recorded compressive strength
values of 1.5–4.0 MPa with 3% cement stabilisation of kaolinitic soils.

Fig. 4. Failure pattern of specimens showing delamination of outer surface.

8 E.B. Ojo et al. / Case Studies in Construction Materials 11 (2019) e00262

Fig. 5. Variation of compressive strength with initial curing temperature for samples tested in the (a) oven-dry condition (b) saturated condition (RT: Room
temperature).

3.5. Effect of water saturation on compressive strength

Evaluation of compressive strength in the saturated condition gives the ‘least’ strength which characterises the lower
bound performance of earth blocks [19]; although, authors have argued that this evaluation condition maybe too extreme for
this class of materials. Despite satisfactory compressive strengths obtained in the oven dry condition, only samples cured
initially at 105
C remained intact to allow testing in the saturated condition. This further signifies the importance of initial
curing temperature to the alkali activation of muscovite rich soils. Clays possess an inherent axial compressive strength in
the dry condition that is lost in the presence of moisture [19]. Hence, a true test of stabilisation of clay particles should be
evaluated using the saturated compressive strength since the inherent strength of dry clay may present a misleading
resistance to compression.
Compared to the oven dry condition, the compressive strength dropped by 83% to 1.82 MPa (Fig. 5b) for samples tested
in the saturated condition yielding a wet strength to dry strength ratio of about 17%. This suggests that the residual
strength observed in the saturated condition can solely be attributed to alkali activation of a fraction of the clays. Also, the
large drop observed may be attributed to the absorption of water by the unreacted clay minerals [34] as well as
development of pore water pressures within the fine grains [19]. Similar reduction in strength has been reported in various
studies where wet strength to dry strength ratio of 20–55% have been recorded for cement stabilised earth masonry
[29,33] and 30% in geopolymer stabilised kaolinitic soils [11]. The presence of unreacted minerals may be attributed to the
low alkaline concentration used in the study. However, average values of 1 MPa have been established as minimum
compressive strength in the saturated condition for unfired earth [23] and values obtained in this study exceed this
minimum specification.

3.6. Effect of additional room temperature curing on compressive strength

Given the low reactivity of uncalcined clay minerals, studies have reported that additional curing at room temperature
allows for continued dissolution of minerals resulting in improved mechanical properties [11]. Additional curing at room
temperature did not reveal statistically significant change in compressive strength for all samples as can be observed in
Fig. 5a. According to Oelkers et al. [35], dissolution of silica and alumina species in muscovite is relatively fast at the initial
stage but subsequently reduces as it reaches a steady state of solution concentration. This would suggest that compressive
strength stabilises at an early age following the attainment of steady state concentration of species, unlike other clay
minerals. Also, additional curing of samples in room temperature from 7 to 15 days of samples cured at 60
C did not improve
their water stability as samples disintegrated after extended curing. The results show that initial curing temperature is a
critical variable compared to additional curing at room temperature in alkali activation of muscovite rich soils.

3.7. XRD analysis

Fig. 6 presents XRD spectra of the starting clay and alkali activated samples cured at vaying initial curing temperatures
and tested after 15 days. The original crystalline phases identified with the starting materials remained after alkali activation
confirming the presence of residual unreacted clay minerals in the mixture. This explains the significant water absorption of
immersed samples which resulted in significant drop in mechanical properties in the saturated condition.
 E.B. Ojo et al. / Case Studies in Construction Materials 11 (2019) e00262 9

Fig. 6. XRD spectra of starting clay and alkali activated clay at different curing temperatures.

XRD analysis did not show clear identification of newly formed phases due to the high background noise and high
crystallinity of unreacted minerals such as quartz and sanidine. It is known that the main reaction products of alkali
activation of low Ca-aluminosilicate systems are typically sodium aluminosilicate hydrate (N-A-S-H) gels which serve as the
main binding phase. These binders exhibit long and medium range disorder making it appear amorphous in XRD spectra
with a broad hump between 25–40 2u [11,36]. But this is typical when amorphous precursors (metakaolin and fly ash) are
used. Other studies have mentioned the presence of new Na aluminosilicate phases (Na-zeolitic minerals and
hydroxysodalite) as products of alkali activation of kaolin and other clay minerals [8,20]. These products of alkali
activation were not identified from the XRD spectra in this study. According to Zhang et al. [37], addition of silicate to
activator solutions significantly reduces crystalline formation leading to a matrix of higher homogeneity in microstructure
and improved compressive strength.
Analysis of the XRD spectra reveals that some changes can be observed around 20–33 2u angles as shown in Fig. 7.
However, given the low reactivity of the precursors and dilute alkaline activator, it is not clear if this is increased background
noise or indication of a formation of weak geopolymer binders. Comparison of muscovite peak shapes for the varying curing
conditions is presented in Fig. 7 and shows a reduction of the characteristic peaks which is indicative of a disruption of
muscovite structure with increase in curing temperature. This is in agreement with studies which have reported an increase
in dissolution of muscovite in alkaline conditions with increase in temperature [38]. The increase in temperature reduces the
activation energy thereby promoting higher rate of dissolution of muscovite minerals leading to improved mechanical
properties. [38]. In addition, increase in alkalinity derived from loss of water at higher curing temperatures leads to a higher
dissolution of muscovite minerals [39]. Similar reduction in peak intensity after alkaline treatment of natural clay minerals
has been reported in other studies [40,41]. According to Kuwahara [42], alkali dissolution of muscovite minerals takes place
primarily at the edge surfaces with little to no reaction taking place at the basal surfaces. This would explain the weak
interactions observed. This further confirms that elevated initial curing temperature is critical to allow significant reaction to
provide sufficient binding in muscovite rich soils as higher temperatures deliver more energy to dissolve alumina and silica

Fig. 7. XRD spectra of starting clay and alkali activated clay at different curing temperatures showing reduction in peak intensity of muscovite minerals (M-
Muscovite, S-Sanidine, Q-Quartz).
10 E.B. Ojo et al. / Case Studies in Construction Materials 11 (2019) e00262

species [10]. This is in contrast to alkali activation of kaolinitic clays, where reactions proceed at room temperature and
elevated curing is restricted to a maximum of 90
C as higher temperatures cause a breakdown of the binding gel phase.

3.8. SEM-EDX characterization

Fig. 8 presents SEM BSE images of internal microstructure from the external surface for samples cured initially at room
temperature and 105
C. Because mechanical characterisation of samples cured at room temperature and 60
C did not show
significant differences, comparative assessment in this section is made between samples cured at room temperature and
105
C only. The micrographs show a heterogeneous microstructure comprising of a binder phase surrounding particles of
varying sizes. Porous nature of microstructure confirms weak reaction between soils and alkali activators under room
temperature curing. This explains the lack of water stability of these specimens as high pore pressures developed would
compromise the structural integrity of these samples. At elevated initial curing temperatures, microstructure appears more
compact with fewer voids.
Irrespective of curing temperature, images show a lateral variation in microstructure; from external surfaces to a depth of
300–400 mm reveal a more compact microstructure relative to the lower strata. This may be attributed to the evaporation of
water during the curing process resulting in concentration gradients and thus difference in reactivity of the clay minerals.
Also, liquid phase migration which is typically observed during extrusion moulding [43] may also result in concentration
gradients within the samples with higher concentrations at the surface relative to the interior parts. Consequently, higher
dissolution rates at the surface relative to the interior parts would result in graded microstructure as observed. Because the
same pattern is observed irrespective of curing condition, it is assumed that the latter (liquid phase migration) that takes
place prior to curing is responsible for this stratification. This also explains the delamination of outer surfaces observed
during axial compression as well as pattern of disintegration when immersed in water.
Higher magnification shows the formation of randomly distributed needle-like phases with a length range of about 3 mm
in samples cured at room temperature and increase in diameter of these phases at higher initial curing temperature (Fig. 9).

Fig. 8. SEM BSE images of samples cured at different temperatures (a) Room temperature (b) 105
C.

Fig. 9. SEM BSE images of samples cured at (a) room temperature and (b) 105
C showing evolution of reaction products with increase in temperature.
 E.B. Ojo et al. / Case Studies in Construction Materials 11 (2019) e00262 11

These products show morphology which is distinct from the surrounding matrix. The formation of secondary products has
been reported extensively in various studies as the binding mechanism obtained in alkali activation [40]. Also, studies on
zeolite synthesis have reported partial dissolution of muscovite substrates into zeolites after alkaline treatment [44]. The
absence of new peaks from XRD spectra would suggest that these precipitates are amorphous or constitutes a minor portion
of the matrix.
EDX analysis was conducted to further elucidate the elemental composition of the alkali activated soils as well as
illustrate elemental distribution to show where elemental combinations and variations exist. Fig. 10 shows BSE images as
well as combined elemental map distribution of major elements for samples cured at room temperature. From the EDX
maps, larger sized particles can be identified by the predominant element composition. For instance, areas enriched in Si
only correspond to quartz particles, whilst regions enriched in Si, Al and K correspond to sanidine particles. These unreacted
quartz and sanidine particles are surrounded by a binder phase. EDX sum spectrum confirms the presence of the following
elements in the system; Silicon, Aluminium, Potassium, Magnesium, Sodium, Iron and Titanium. With increased initial
curing temperature, combined elemental map distribution shows a more defined distribution of elements within the system
(Fig. 11). This clearly elucidates increased dissolution of these species with increase in temperature and possible
polymerisation of these species.
EDX analysis was used to disclose the composition of the newly formed phases not clearly identified by XRD (Fig. 12).
Higher magnification of binder phase of samples cured at 105
C reveals a silicon rich system with Al and Na distributed
throughout the phase. Whereas, these elements (Si and Al) appear to be evenly distributed within the binder phase, Na
element distribution appears to be concentrated in some regions. The orientation of Na rich regions in the map appear to be
consistent with orientation of reaction products observed in the BSE images indicating Na to be a major constituent of these
phases. Furthermore, distribution of these sodium rich regions show that these products are absent in regions corresponding
to the presence of larger quartz and sanidine particles. The absence of voids in positions where these products occur in other
single elemental maps indicate composition of products to include Si and Al in addition to Na. The surrounding areas in the
binder phase are therefore presumed to be unreacted muscovite minerals suggesting that this newly formed phase is
presumably a reaction product of muscovite associated with alkali activation. The absence of new crystalline peaks in the
XRD spectra suggest that these phases formed are Na-aluminosilicates which are amorphous or poorly crystalline. This is
identified on the basis of elemental composition data only.

Fig. 10. BSE images and EDX maps of Microstructure for samples cured at initial curing temperature of 105
C (Key for element map: Silicon-Red, Aluminium-
Green, Sodium-Blue).
12 E.B. Ojo et al. / Case Studies in Construction Materials 11 (2019) e00262

Fig. 11. BSE images and EDX maps of Microstructure for samples cured at initial curing temperature of 105
C (Key for element map: Silicon-Red, Aluminium-
Green, Sodium-Blue).

Fig. 12. Mixed Element map and single element map of samples cured at 105
C showing elemental composition of reaction products. (Key for element map:
Silicon-Red, Aluminium-Green, Sodium-Blue).
 E.B. Ojo et al. / Case Studies in Construction Materials 11 (2019) e00262 13

Fig. 13. FTIR Spectra of alkali activated sample (cured at 105
C) and pure muscovite mineral.

3.9. FTIR characterization

In order to further characterise newly formed phases observed from SEM/EDX analysis, Fig. 13 presents FTIR spectra of
pure muscovite mineral and alkali activated samples cured at 105
C only. FTIR spectrum of muscovite mineral is dominated
by a Si-O-Al band at 975 cm1. On the other hand, dominant band in the activated sample is broader with a higher intensity
and is located at a higher wavenumber (1031 cm1). Studies by Prud’homme et al. [45] have shown that total displacement of
main band during the formation of geopolymers is approximately 40 cm1 to a position which corresponds to 940 cm-1. This
is attributed to asymmetric stretching of Si-O-Si and Si-O-(Al) vibration bonds [20,46,47]. However, larger main band
displacement (56 cm1) observed in this study can be attributed to the formation of aluminosilicate gels with Na [45]. Due to
the low reactivity of the precursors as well as low alkalinity of solutions, weak concentration of Si and Al species in the
system would inhibit the polycondensation reaction and consequently, network formation [45]. This explains the absence of
new peaks or characteristic geopolymer ‘hump’ in the XRD spectra. This also confirms structural alteration of muscovite as
observed with XRD spectra. Similar behaviour has been reported with alkali activation of uncalcined illite [48]. The
stretching vibration absorption peaks of O H and H-0OH can be observed at 3447 and 1636 cm1 and confirm the
presence of chemically bound water [46] in the uncalcined soil. FTIR spectra also shows slight carbonate bands associated
with atmospheric carbonation of unconsumed NaOH in the system. These carbonates are typically associated with low
reactive precursors such as natural clays [48]. Evidence confirms results from XRD which indicate no significant amount of
carbonates were formed due to low molarity of alkali activators used.

4. Conclusions

This study explored the feasibility of producing more environmentally friendly building materials from natural
aluminosilicate minerals present in soil using low concentration alkali activator solutions. Small scale samples were
produced using extrusion moulding and subjected to different curing regimes to ascertain the effect of initial curing
temperature as well as curing duration on the alkali activation and consequent strength development in muscovite rich soils.
Literature is scarce on the alkali activation of the natural muscovite rich soils; this study has provided some insight on
behaviour of such minerals in low concentration alkali activator solutions.

 The results reveal alkali activation of these clays to be a satisfactory mechanism for the stabilisation of these soils and was
evident in the impressive mechanical properties obtained in the dry state relative to other stabilisation mechanisms.
These materials may be suitable for load-bearing masonry applications.
 In the saturated condition, sufficient binding for the production of water stable units was achieved only at elevated initial
curing temperatures of 105
C for 5 h revealing the temperature dependence of the process. This suggests that the scope of
application of building units may be expanded to moisture susceptible environments with proper optimisation of initial
curing temperature. Physical properties (water absorption) of samples cured at this temperature are comparable to fired
bricks.
 Analysis of XRD spectra shows muscovite minerals undergo significant structural changes following treatment with
diluted alkali activators whilst other minerals (quartz and sanidine) remain largely unreactive.
14 E.B. Ojo et al. / Case Studies in Construction Materials 11 (2019) e00262

 Porous and graded microstructure reveal limitations associated with extrusion moulding and suggest that optimisation of
moisture content during moulding will result in enhanced packing density and consequently improved mechanical and
physical properties.
 SEM-EDX/FTIR analysis reveal the formation of phases which are presumably Na-aluminosilicatesgels formed as a result of
a dissolution of muscovite and are responsible for the binding observed. The variation of the formation of precipitates with
increasing curing temperature further confirm the need of higher temperatures to facilitate the dissolution of alumina and
silica species from natural aluminosilicates.

This study has demonstrated the use of elevated temperature curing conditions with low akali concentrations as a more
eco-friendly route for the development of low impact building materials. The results show the binding provided with low
molarity alkali solutions is sufficient for water stable units and serves as a basis for further research for the use of this
technology in regions where muscovite minerals are predominant.

Acknowledgements

The authors gratefully acknowledge the financial support given by the Pan African Materials Institute (AUST/PAMI/2015
5415-NG) under the World Bank African Centres of Excellence Program as well as the Brazilian National Council for Scientific
and Technological Development (Conselho Nacional de Desenvolvimento Científico e Tecnológico) PQ CNPq 307723/2017-8/
& PDJ CNPq 409538/2017-5).

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 Update
Case Studies in Construction Materials
Volume 14, Issue , June 2021, Page

DOI: https://doi.org/10.1016/j.cscm.2021.e00486
 Case Studies in Construction Materials 14 (2021) e00486

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previous volumes of Case Studies in Construction Materials. Hence, the authors of the below articles were contacted after
publication to request a Declaration of Interest statement:

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2214-5095/© 2021 The Author(s). Published by Elsevier Ltd. All rights reserved.
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