Journal of Environmental Management 321 (2022) 115980

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Journal of Environmental Management

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

Research article

Microstructural and compaction characteristics of tropical black clay soil

subgrade modified with lead-zinc mine tailings
Adegboyega Oduniyi Odumade a, *, Fidelis O. Okafor b, Chijioke Christopher Ikeagwuani b
a
Civil Engineering Department, Alex Ekwueme Federal University, Ndufu-Alike, Nigeria
b
Civil Engineering Department, University of Nigeria, Nsukka, Enugu State, Nigeria

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

Keywords: Lead–Zinc Mine tailings (LZMT) are wastes generated after the extraction of lead and zinc from mined mineral
Expansive soil ore, whose disposal mechanism is gradually becoming environmentally unfriendly. For effective recycling of
Fractals LZMT, this present study utilized a combination of LZMT and Portland limestone cement (PLC) to improve the
Image segmentation technique
compaction and microstructural characteristics of tropical black clay soil (TBCS) for use in pavement design and
Microstructural analysis
construction. The LZMT and PLC were added to the expansive soil in varying proportions with mix ratios
Lead–zinc mine tailing
Stabilization generated from Taguchi orthogonal array. The result obtained for the compaction characteristics showed that the
maximum dry density (MDD) increased significantly when a combination of 20% LMZT and 4% PLC were
blended with the expansive soil. The increase in the MDD was attributed to the formation of cementitious
compounds. In addition, the optimum mix ratio obtained from the unconfined compressive strength of the TBCS,
was used for the evaluation of the pore structure characteristics which included porosity, tortuosity and
permeability. The result obtained from the analysis that was implemented with a combination of fractal ge­
ometry and Bradley and Roth adaptive thresholding image segmentation technique, indicates the possibility of a
slight reduction in the strength properties of the modified soil due to its high level of porosity. Also, the
permeability and tortuosity values obtained from the present study suggest a slight increase in the permeability
of the modified soil-additive mixtures which may not be unconnected to the occurrence of pozzolanic reaction
that resulted in the agglomeration and flocculation of the LZMT-PLC modified TBCS. Furthermore, microstruc­
tural analysis was executed on the modified TBCS and LZMT using Fourier transform infrared spectroscopy
(FTIR) and scanning electron microscopy (SEM). The result from the FTIR analysis indicates the pozzolanic
character of LZMT in the presence of Si–O and Al–O tension bond with the bonds around 1000 cm− 1 wave­
number, while the SEM analysis reveals the formation of a cementitious compound in the modified expansive
soil-LZMT-PLC mixture.

1. Introduction
1.1. Overview of mine tailing
Mine tailings are solid industrial residue from extractive or mining
industries. They are the valueless fraction remaining when the desirable
or priceless fraction has been extracted from an ore. They have varying
shapes and sizes which depend on the method deployed during the
mining operation of the ore (Sahu et al., 2014). They consist of slurry or
mud-like material that comprises both coarse and fine particles. The
coarse particles, more often than not, constitute about 40–50% of the
total mine tailings, and they are frequently utilized in landfills (Chen
et al., 2020). The fine particles, which have sizes less than 20 μm, are
disposed of in tailing ponds apparently due to their adverse effect on
workability and landfills (Deng et al., 2018).
Generally, the chemical compositions of mine tailings are similar to
that of the parent ore from which the tailings are generated. Some of the
chemical constituents include heavy metals and sometimes, toxic re­
sidual reagents from the mining operation or the extraction of the
desired material of the mineral ore (Mahmood and Mulligan, 2010).
Descriptively, the heavy metals are metalloids or metals whose densities
are greater than 5 g/cm3, such as cadmium (Cd), arsenic (As), zinc (Zn),
lead (Pb) and mercury (Hg) (Kan et al., 2021a). They are largely known
to be stable and very difficult to degrade or neutralize physically. They

* Corresponding author.
E-mail addresses: adeodumade00@gmail.com (A.O. Odumade), fidelis.okafor@unn.edu.ng (F.O. Okafor), chijioke.ikeagwuani@unn.edu.ng (C.C. Ikeagwuani).

https://doi.org/10.1016/j.jenvman.2022.115980
Received 22 April 2022; Received in revised form 25 July 2022; Accepted 6 August 2022
Available online 21 August 2022
0301-4797/© 2022 Elsevier Ltd. All rights reserved.
A.O. Odumade et al.
exist in different forms like fluoride, chloride and sulphate (Chen et al.,
2009). Their concentration varies greatly and sometimes, they may
exceed the permissible limit within an environment. They have been
widely reported to cause grievous environmental problems to humans
and also to endanger the equilibrium of fauna (Katsioti et al., 2008).
They are also known to be carcinogenic and mutagenic.
Furthermore, most heavy metals present in the mine tailings have the
capacity to bioaccumulate in the human body system resulting in bio­
logical and physiological complications. For example, LZMT that
contain Pb have been reported to cause severe damage to the human
nervous system due to lead poisoning (Kan et al., 2021; Silver et al.,
2016; Ebrahimi et al., 2020). In addition, LZMT that contain elevated
concentration of some highly toxic metals such as Cd and Zn, have also
been reported to adversely affect geochemical environment (Ye et al.,
2002; Igwe et al., 2017; Ugwu et al., 2022). The toxic metals migrate to
the geochemical environment, which are surface water and under­
ground water, and increase the concentration level of the toxic metals in
it thereby rendering it unsafe for human and animal consumption.
Similarly, large quantity of LZMT that contain pyrite or some other
forms of sulfide may react with oxygen and water to produce sulphuric
acid. The produced sulphuric acid could facilitate the infiltration or
leaching of some heavy metals present in the mine tailings. In addition,
the produced sulphuric acid may diffuse into the surrounding atmo­
sphere leading to the formation of haze and acid precipitation that may
result in severe environmental pollution, land degradation and reduced
arable land which are highly disturbing (Chen et al., 2014; Zhuang et al.,
2009; Liu et al., 2017).
Even more disturbing is that crops cultivated on such heavy metal
polluted environment within the vicinity of the mining site can easily
ingest and accumulate the heavy metals present in the mine tailings
leading to potential health risk for humans that depend on them as their
source of food (McBride, 2007; Yang et al., 2022). Substantial evidence
has proven that an environment contaminated with heavy metals results
in severe health complications to the local inhabitants that reside around
that environment (Zhuang et al., 2009; Igwe et al., 2014, 2017). In
addition, the aquatic lives present in the rivers or streams within the
contaminated environment are also affected due to constant exposure to
the heavy metals. Unsurprisingly, mine tailings that contain heavy
metals, despite their enormous quantity generated worldwide, have
limited applications in practice apparently due to their adverse effect on
the environment. Hence, the need to develop effective and pragmatic
ways that can effectively be utilized in practice to ameliorate the adverse
effect of mine tailings cannot be overemphasized.
Interestingly, different approaches have been suggested by
numerous researchers for the amelioration of the adverse effect of heavy
metals. These approaches are broadly grouped into three. The first
approach involves the utilization of a process known as capping to
isolate the mined residue from the nearby environment. The second
approach involves blending the mine-tailings with cementitious mate­
rials or chemicals to stabilize them chemically. This approach usually
results in the immobilization of the heavy metals contained in the mine
tailings. The third approach involves the simultaneous utilization of the
first and second approaches. Remarkably, the second and the third ap­
proaches are the most widely used methods because they can effectively
result in the solidification/stabilization of the heavy metals in the mine
tailing thereby leading to its sustainable disposal. The solidification/
stabilization process has an advantage which is that it ensures that the
heavy metals in the mine tailings are converted into more chemically
and physically stable forms such that their ability to affect the envi­
ronment adversely is drastically reduced (Chen et al., 2009).
This singular advantage of the solidification/stabilization process
has promoted its utilization in practice, particularly in concrete and
bricks production (Surendra et al., 2007; Ghazi et al., 2022). The
properties of bricks or concrete produced with mine tailings are, in most
cases, found to be better than those produced without mine tailings. In
addition, the bricks or concrete produced with mine tailings are found to
2
Journal of Environmental Management 321 (2022) 115980
be economical. In recent years, few highway and geotechnical research
engineers have started exploring this rare advantage derivable from the
solidification/stabilization process to advance the course of mine tail­
ings utilization in the construction of pavement. Ojuri et al. (2017), in a
study on the utilization of mine tailings for pavement design and con­
struction, used a combination of mine tailings and a binary binder,
lime-cement, to improve the properties of a weak lateritic soil subgrade.
The binary binder which was proportioned in the ratio of 1:2, was
thoroughly blended and added with varying proportions of mine tailings
and lateritic soil to form a homogeneous mixture. The results obtained
from the study reveal clearly that mine tailings when blended with weak
lateritic soil enhances its properties.
In a related study, Tong et al. (2021) utilized iron tailings, one of the
available mine tailings on earth, to improve the strength properties of
highly plastic soil. The iron tailings were blended with the soil in the
presence of cement and its effect on the strength properties were eval­
uated after the mixture was subjected to various days of curing ranging
from 0 to 90 days. The result from the study showed that there was a
significant increase in the strength properties of the soil that was
admixed with the iron tailings and cement. In addition, there was a
corresponding increase in the strength properties of the soil as the curing
days increased. In the same vein, Etim et al. (2017) used a combination
of lime and iron tailings to alter the chemical composition of an
expansive soil for its overall strength improvement. The strength prop­
erties, which included UCS and CBR, were greatly improved when a
combined 8% lime and 10% iron tailings were blended thoroughly with
the soil by its air-dried weight and made to cure for a duration of 28
days. The improvement in the strength properties of the soil was
adduced to the pozzolanic reaction experienced between the additives
(lime & iron tailings) and the expansive soil. Other researchers who have
also used mine tailings for soil subgrade improvement and obtained
similar results include Yohanna et al. (2021) and Osinubi et al. (2015).
From the foregoing literature on the utilization of mine tailings for
the improvement of pavement material, it is apparent that only very
little attempt have been made to adequately evaluate the microstruc­
tural and compaction characteristics of mine tailings-modified soil
especially expansive soil that is widely known to be problematic
(Ikeagwuani and Nwonu, 2019, 2021a; Soltani and Estabragh, 2015;
Syed et al., 2021; Al-Taie et al., 2018; Jalal et al., 2021; Zimar et al.,
2022a). This present study, therefore, evaluates the microstructural as
well as compaction characteristics of an expansive soil modified with
lead-zinc mine tailings (LZMT), a mine tailing obtained from a mining
industry. Most of the microstructural characteristics of the mine tailings
modified expansive soil were evaluated using the image segmentation
technique.
It is worth stating at this juncture that expansive soil, which is the
soil considered for improvement with LZMT in this study, is highly
characterized by contraction and expansion phenomena. It exhibit sig­
nificant volumetric change when subjected to moisture variation. The
volumetric change, which negatively affects the engineering properties
of the soil, is prevalent in wet and dry seasons. In wet season, it absorbs
moisture leading to an increase in the volume of the soil; while in dry
season the absorbed moisture dissipates leading to a reduction in its
volume (Nwonu and Ikeagwuani, 2021). This eventually results in
visible surficial cracks on the expansive soil. In addition, the volumetric
change of the expansive soil impacts negatively on structures con­
structed on it. The failures of most structures constructed on the soils are
rife in the literature (Ikeagwuani, 2021; Ijaz et al., 2020; Zimar et al.,
2022b; Yu et al., 2014). Hence, it is imperative to find economical
remedial measures to improve the soil so that it can be safely used for
not just pavement construction purposes but also for other engineering
and hydraulic purposes such as the construction of earth dams, em­
bankments, retaining walls, etc.
A.O. Odumade et al.
1.2. Image segmentation
Image segmentation is an integral concept in the digital processing of
image. It is a process whereby an input image is separated into various
segments or homogeneous regions. Put succinctly, it is a technique that
is utilized to partition an image into a different disjoint but meaningful
set of images that possesses identical features and properties (Gonzalez
and Woods, 2002; Solomon and Breckon, 2010). Its core objective is for
simplification and facilitation of easy analysis and comprehension of
images. It is an essential technique that has been employed in several
fields of discipline for pattern recognition, video surveillance, automatic
traffic control systems, number plate identification, medical imaging,
image-based search and so on. There are different types of image seg­
mentation techniques, and they have been broadly grouped into seven
categories namely, thresholding-based segmentation, edge-based seg­
mentation, region-based segmentation, clustering-based segmentation,
watershed-based segmentation, partial differential equation-based seg­
mentation and neural network-based segmentation (Pal and Pal, 1993).
Notably, only the first image segmentation technique, the
thresholding-based segmentation technique, was considered in the
present study due to its simplicity.
1.3. Thresholding-based segmentation technique
The thresholding-based segmentation is a technique used to detect
an object in an image using threshold value(s). They are the simplest and
most widely used method of image segmentation technique. The tech­
nique involves the extraction of an object (foreground) from the back­
ground of an input image (Huang and Wang, 1995). The extraction is
implemented by dividing the intensity of the picture element (also called
pixels) of the input image into foreground and background with a
certain specified value known as threshold. It is frequently utilized
whenever the intensity of the object of an input image exceeds that of
the background. Broadly, there are three thresholding-based segmen­
tation techniques. They are the global, variable and multiple thresh­
olding segmentation techniques.
The first thresholding method, the global thresholding technique
(known loosely as a fixed thresholding method), uses a fixed threshold
value, T for the analysis of an entire input image, k(x, y) to generate a
binary output image, g(x, y), which is expressed as:
{
1, k(x, y) > T
g(x, y) = (1)
0, k(x, y) < T
where, x is the number of rows of pixel of an image and y is the number
of columns of an image.
The second thresholding method, the adaptive thresholding seg­
mentation technique, is a method that computes different thresholds for
every pixel in an input image. It is a robust thresholding technique
because it takes into account variations in illumination that varies
spatially. The threshold value is a function of x and y. There are quite a
number of adaptive thresholding techniques that have been developed
for image segmentation, and quite a few of them have been applied
successfully for the segmentation of images in diverse fields.
The last thresholding method, the multiple thresholding, is a tech­
nique that has more than one threshold values such as T0 and T1 in its
algorithm as the name suggest. Given an input image, g(x, y) that uses
multiple thresholding technique for its analysis of an input image, the
relationship between the input image and the output image, k(x, y) can
be expressed as:
⎧
⎨ m k(x, y) > T1
g(x, y) = n k(x, y) ≤ T1 (2)
⎩
0 k(x, y) ≤ T0
where, m and n are any specified pixel values.
3
Journal of Environmental Management 321 (2022) 115980
1.4. Characterization of pore structure
For effective characterization of pore structure of SEM images, the
concept of fractals, which was given fillip by Benoit Mandelbrot (1967)
needs to be expatiated. This is because SEM images, like most natural
objects, have jagged and complex structures that makes their description
difficult with the use of simple primitive (Wu et al., 2020; Mandelbrot,
1983; Chaudhuri and Sarker, 1995). In fact, most natural objects that are
found in several fields of study such as geophysics, geography and ge­
ology possess the characteristics of fractals (Amosu et al., 2018; Li et al.,
2009; Pentland, 1984). For this reason, the concept of fractals or fractal
geometry, which is used frequently to characterize the pore structure of
SEM images, needs proper explanation as mentioned earlier.
1.5. Fractal and box-counting technique
The concept of fractal or fractal analysis was expounded by a French
mathematician, Mandelbrot, in his now famous paper titled, How long is
the coast of Britain? Statistical self-similarity and fractional dimension
(Mandelbrot, 1967). It is a concept that emanated from the coastline
paradox whereby the dimension of a coastline is highly deceptive
because of its tendency to appear somewhat easy to measure at first sight
but difficult when attempts are made to measure it physically. In fact, its
measurement from practical evidence has shown that it depends on the
length of the “ruler” used for measuring it. Most natural objects, like the
length of a coastline, have dimensions that are very difficult to measure
with Euclidean geometry due to their erratic and complex nature (Xu
and Weng, 2006; Mandelbrot, 1982). Lewis Richardson (1961), one of
the earliest researchers who contributed to the concept of fractals,
developed a mathematical expression for determining the dimension of
a coastline. The mathematical expression, which is expressed as shown
in Equation (3), involves a relationship between the length of coastline,
L(G) and the length of ruler, G.
L(G) = MG1− Df
(3)
where, M is a positive proportionality constant and Df is known as
fractal dimension or Hausdorff dimension or sometimes as Hausdorff-
Besicovich (Buczkowski et al., 1998).
The fractal dimension (Df ) in Equation (3) is a number that indicates
the complexity of a coastline. The higher the fractal dimension of a
coastline, the more complex the coastline is. However, it is very difficult
to determine fractal dimension directly. In fact, the earliest method
(walker’s rule or divider rule method) developed by Richardson is barely
used in practice because it is fraught with limitations (Gonzato, 1998).
Interestingly, several algorithms have been developed for deter­
mining fractal dimension but the widely used algorithm is the
Minkowski-Bouligand box-counting dimension method because of its
simplicity and computational efficiency. The Minkowski-Bouligand box-
counting dimension or simply the box-counting method is a very simple
technique that involves the recognition of each instance of a particular
feature wherever it is found in an image to be analyzed and then super-
imposing or “covering” such feature with boxes that have different sizes.
The number of boxes that covers the feature of interest in the image
being analyzed is subsequently counted and the value obtained is used to
estimate the fractal dimension (Df ), with the expression shown in
Equation (4):
N = C(1/r)Df (4)
where; N represents the number of boxes with a side length of r and C is
the proportionality constant.
Equation (4) can be transformed as:
logN = logC(1/r)Df (5)
The box-counting fractal dimension is often determined through the
A.O. Odumade et al. Journal of Environmental Management 321 (2022) 115980

least square method with the linear expression: Table 1

Properties of the TBCS, LZMT and PLC.
Y = Df ​ x ​ X + B (6)
S/N Properties TBCS LZMT PLC
where, Y represents logN and X represents log(1 /r). Df is the slope of the 1 Specific gravity 2.29 2.86 2.98
straight line and B, which is the intercept, represents logC. 2 % Passing BS No. 200 test 64.8 50 –
sieve
3 Natural moisture content 23.4 – –
1.5.1. Integration of fractal dimension to pore structure characteristics and (%)
size parameters 4 Liquid limit 58.2 – –
It has been demonstrated by several researchers that pore space, 5 Plastic limit 29.8 – –
which is different geometric parameters, can be effectively explained 6 Plasticity index 28.4 – –
7 Swelling potential Medium
with fractals (Jobmann and Billaux, 2010; Pape et al., 1987a). The
– –
8 OMC BSL 21.78% – –
geometric parameters of pore space include pore radius, tortuosity and WAS 20.02%
porosity, and they govern the processes of pore space transport such as BSH 18.86%
fluid flow and the diffusion of components dissolved in the fluid (Katz 9 MDD BSL 1.57 g/cm3 – –
and Thompson, 1985). In another development, it has been demon­ WAS 1.60 g/cm3
BSH 1.65 g/cm3
strated that pore geometry can be described suitably with the pigeon­ 10 AASHTO classification A-7-6 (24) – –
hole model introduced in the year 1984 by Pape et al. (1984). In the 11 USCS classification CH – –
following years, Pape et al. (1999) developed a relationship between 12 NBRRI classification Medium swell potential – –
pore geometry and permeability with the pigeonhole model. The 13 Subgrade class designation S1 – –
14 CBR (%) Unsoaked 5.33
pigeonhole model comprises two sets of spheres. One set represents
– –
Soaked 2.15 – –
grain while the other set represents pores. The radius of the spheres 15 UCS 98.07 kN/m2 – –
representing grain and pores are usually written as rgrain and rsite 16 Colour Grayish - black Deep Ash Grey
respectively. Both set of spheres form a cascading hemispherical
sub-structure. In addition, the pores in the pigeonhole model are con­
nected by small channels that are explained by effective hydraulic radius Table 2
reff of a corresponding capillary. The three radii reff , rsite and rgrain Oxide composition of the TBCS, LZMT and PLC.
mentioned in the pigeonhole model are referred to as the porous me­ Compounds TBCS (%) LZMT (%) PLC (%)
dium size parameters. They are connected by an empirical relation
SiO₂₂ 59.548 35.144 19.16
developed by Pape et al. (1984). The empirical relation, which has been
CaO 1.0466 2.598 64.25
confirmed by Pape et al. (1999), is expressed as: Al₂₂O₃₃ 16.071 9.704 4.92
( )c Fe₂₂O₃₃ 7.2158 9.0353 0.75
/ /
rgrain r = rgrain r (7) MgO 3.28 2.41 2.17
site eff SO₃₃ 0.1320 1.1199 1.02
K₂₂O 0.8900 1.1159 0.35
where c is the structural coefficient. P2O5 0.2756 0.1747 –
TiO2 0.9842 0.2992 –
MnO 0.6697 2.5630 –
1.6. Relationship between permeability and porosity CuO 0.0262 0.00784 –
ZnO 0.01480 1.0219 –
The well-established Kozeny-Carman expression for estimation of
permeability from a porous medium or pore size parameters is given as
(Carman, 1997; Kozeny, 1927): ( )(D− 3) ( )c(D− 3)
/ /
/ ∅ = 0.5 rgrain r = 0.5 rgrain r (13)
2
k = reff 8F (8) site eff

where F is the formation factor introduced firstly by Archie (1942). It is 2. Methodology

expressed as the ratio of tortuosity, F and porosity, ∅ .
2.1. Materials
F = T/∅ (9)
2.1.1. Tropical black cotton soil
Substituting Equation (2) into (1)
Tropical Black cotton soil (TBCS), an expansive soil, obtained within
/
2
k = reff ∅ 8T (10) the Northern-Eastern axis of Nigeria, specifically, from Taraku - Naka –
Agagbe in Benue State, Nigeria (7◦ 37′ 39′′ N, 8◦ 13’ 34” E) was used for
According to Pape et al. (1987b), the tortuosity behaves like a fractal this investigation. The geology of the area indicates little variation in
and it relies on fractal dimension, Df and the ratio of reff and rgrain . It is rainfall intensity and soil properties, which is typical of soils found in
given as: most tropical countries (Odumade et al., 2019). The TBCS were collected
at a depth of 1.5 m below the ground surface using the disturbed sam­
( )2(D−
pling technique.
2)
/
T = 1.34 rgrain r (11)
site

Inserting Equation (7) into (11), we obtain 2.1.2. Lead-zinc mine tailing
( )2c(D− The lead-zinc mine tailing was obtained from First Patriot Limited, a
mineral ore mining company located at Enyigba, Ikwo, Ebonyi state,
2)
/
T = 1.34 rgrain (12)
reff Nigeria. The lead–zinc mine tailing, as noted in the introduction section,
is a residue from the extraction of lead-zinc mineral ore. It was collected
Furthermore, according to Pape et al. (1984), the porosity is related
in slurry form; as such, it was allowed to dry in a humidity-controlled
to the pore size parameter with this expression:
environment for seven days prior to usage. The physical and chemical
properties of the lead-zinc mine tailing are displayed in Tables 1 and 2

4
A.O. Odumade et al. Journal of Environmental Management 321 (2022) 115980

Table 3 technique. Both the FTIR and SEM image analysis were performed on the
Layout of Taguchi orthogonal array and UCS values. optimal mix ratio sample and then compared with that of the FTIR and
Experimental Designation LZMT PLC Coded UCS (kN/ SEM image of the natural TBCS. Notably, the FTIR test is an alternative
runs (%) (%) Unit m2) and a more recent test intended to determine the level of absorption of
A B the constituents of a given material and also to establish the group such
material belongs to. The FTIR spectra of the TBCS and LZMT were
1 T1 5 4 1 1 261.86
2 T2 5 8 1 2 385.38
recorded with a Happ – Genzel spectrometer considering absorption
3 T3 5 12 1 3 503.95 spectra on a wavenumber range varying from 650 cm− 1 – 4000 cm− 1
4 T4 10 4 2 1 358.20 with a resolution of 4 cm− 1.
5 T5 10 8 2 2 469.37
6 T6 10 12 2 3 595.85
2.2.2. Compaction test
7 T7 15 4 3 1 390.10
8 T8 15 8 3 2 512.87 As stated earlier, the compaction test was conducted to determine
9 T9 15 12 3 3 645.83 the maximum dry density (MDD) and optimum moisture content (OMC)
10 T10 20 4 4 1 444.66 of the natural TBCS sample as well as that of various mixes of TBCS and
11 T11 20 8 4 2 543.48 LZMT generated with the mixed-level L18 Taguchi orthogonal array.
12 T12 20 12 4 3 672.92
13 T13 25 4 5 1 450.24
British standard light compaction (BSL), whose procedure is outlined in
14 T14 25 8 5 2 535.20 BS 1377 part 4, 1990, was used to conduct the compaction test. The BSL
15 T15 25 12 5 3 675.12 method involves the use of a rammer weighing 2.5 kg for its compaction.
16 T16 30 4 6 1 412.60 The rammer is allowed to fall freely under its weight from a height of
17 T17 30 8 6 2 520.00
300 mm on samples placed in three layers in a 1000 cm3 mould. Each
18 T18 30 12 6 3 650.50
layer is constrained to receive 27 blows from the freely-falling 2.5 kg
rammer.
respectively. It is evident from Table 2 that the lead–zinc mine tailing,
which was classified as Class C pozzolana (ASTM C618-78, 1978), has 2.2.3. Characterization of pore structure of SEM image
certain pozzolanic properties that can aid in the improvement of the To determine the pore structure characteristics of the SEM image, the
engineering properties of TBCS. following two steps were meticulously followed.
Step 1.
2.1.3. Portland limestone cement Firstly, the original SEM images, which are grayscale, are trans­
The binder utilized in the present study was Portland limestone formed into binary images using the Bradley and Roth adaptive
cement (PLC). It was selected because of its availability in the study area thresholding image segmentation technique (Bradley and Roth, 2011).
as well as its high pozzolanic potential in soil stabilization scheme as The technique, which is also known as the mean method, is an extension
demonstrated in numerous literatures (Odumade et al., 2019). It was of the Wellner’s adaptive thresholding technique (Wellner, 1993). It
obtained commercially from Ebonyi state, Nigeria. Its physical proper­ consists of two phases. The first phase involves computing the integral
ties are displayed in Table 1 while its chemical properties determined image (summed-area table) from the input grayscale image while the
using EDXRF analyzer is presented in Table 2. second phase involves calculating the mean of the s by s pixel using the
already computed integral image for every pixel. The calculated mean of
2.2. Methods the s by s pixel is later compared with that of the current pixel value t, to
determine whether it (current pixel) should be set as black or white in
2.2.1. Experimental procedure the output binary image. The entire operation in Step 1 is executed in
The experimental mix design was performed using L18 mixed-level MATLAB (2020a) software.
Taguchi orthogonal array (Table 3) generated with MINTAB software. Step 2.
In the Taguchi orthogonal array, three levels (4, 8 and 12%) were Shortly after transforming the grayscale image to a binary image, its
assigned to the PLC while six levels (5, 10, 15, 20, 25 and 30%) were pore structure characteristics were determined. This was done by uti­
assigned to the LZMT. Thereafter, a compaction test, which is described lizing the box counting method to obtain the fractal dimension of the
in the next section, was performed to determine the compaction char­ pores (Equation (4)). The obtained fractal dimension was then utilized
acteristics of the TBCS and that of various mixes of the combination of to evaluate the pore characteristics of the binary image with the ex­
TBCS and LZMT generated with the mixed-level L18 Taguchi orthogonal pressions of the pore structure characteristics given in Equations (10),
array. The compaction characteristics determined include the optimum (12) and (13). They include expressions for permeability, k (Equation
moisture content (OMC) and the maximum dry density (MDD). (10)), tortuosity, Ts (Equation (12)), and porosity, ∅s (Equation (13)).
Subsequently, the UCS test, which was executed in accordance with The entire operation involved in this Step 2 is executed with Geo­
BS 1377 part, 1990 (British Standard Institute, 1990b), were conducted BoxCount program. The GeoBoxCount program was written by Amosu
for the natural TBCS and that of the other mix ratios of the combination et al. (2018) in MATLAB (2017b) software. It has a graphical user
of TBCS and LZMT generated with the mixed-level L18 Taguchi interface for easy visualization of the analysis.
orthogonal array. The samples used for the UCS tests were prepared with 3. In order to effectively evaluate the pore structure characteristics,
their various OMC. Shortly after preparing the samples, they were the structural coefficient, c, was taken as 0.39. This is the value rec­
subjected to 28 days of curing in a humidity-controlled environment and ommended by Pape et al. (1984) for sedimentary rock. For the ratio
/
their UCS values were estimated thereafter utilizing the UCS testing between the grain radius and the effective hydraulic radius, rgrain r , the
eff
machine. value 2.9 was adopted. The 2.9 value was adopted because it is the
Furthermore, the optimal mix ratio that gave the highest UCS value
recommended value by Carman (1956) for grains with loose packing.
from the various UCS test conducted on all the samples was later sub­ Similar assumption, which is that the soil grains are loosely packed, is
jected to microstructural analysis tests. The microstructural analysis
made in this study. Lastly, the radius of the grain used in this study for
tests performed on the optimal mix ratio include scanning electron mi­ the determination of the pore characteristic was 1/256 mm (3.906.25
croscopy (SEM) and Fourier Transform Infrared Spectroscopy (FTIR).
nm).
The FTIR was used to establish the absorption level and the chemical
bonds present in the samples while the SEM image was used to deter­
mine the pore structure characteristics through the image segmentation

5
A.O. Odumade et al.
Fig. 1. Relationship between the MDD and LZMT at different PLC content.
Fig. 2. Relationship between the OMC and LZMT at different PLC content.
3. Results and discussion
The results of the preliminary experiment conducted on samples of
the natural TBCS are displayed in Table 1. As shown in Table 1, more
than 50% of the total 500 g natural TBCS sample used for the particle
size distribution passed through the BS No. 200 test sieve which implies
that the soil is composed largely of fine-grained soil. Also from Table 1,
both the liquid and plastic limits of the TBCS determined with Casa­
grande’s instrument (British Standard Institute, 1990a), were found to
be 58.2 and 29.8% respectively.
Furthermore, the plasticity index of the soil, which is simply the
numerical difference between its liquid and plastic limits, was recorded
as 28.4%. This value indicates a very high plasticity (Arora, 2003;
Ikeagwuani and Nwonu, 2020, 2021b). The California bearing ratio
(CBR) test (Bristish Standard Institute, 1990) performed on the natural
TBCS that was classified as A-7- (24) using the American Association of
state highway and official (AASHTO) classification system, revealed that
the unsoaked and soaked CBR values were 5.33% and 2.15% respec­
tively. These unsoaked and soaked CBR values of the natural TBCS fell
short of the minimum recommended value for a material to be used as
subgrade based on the Nigerian general specification for roads and
bridges guidelines (Nigeria General Specification, 1997; Ikeagwuani
et al., 2020). The guideline clearly states that for a material to be used as
subgrade in pavement construction, its unsoaked and soaked CBR values
should not be less than 10% and 5% respectively. This implies that the
unsoaked and soaked CBR of the natural TBCS in this study fell short of
6
Journal of Environmental Management 321 (2022) 115980
the stipulated guideline by as low as 46.7% and 57.0% respectively.
Lastly, the oxide composition analysis performed on a representative
TBCS sample with Energy Dispersive X-ray Fluorescence (EDXRF)
analyzer, revealed that the soil consists largely of silica (59.8%) and
some other trace compounds as displayed in Table 2.
3.1. Compaction
The results of the compaction characteristics are presented in Figs. 1
and 2. Fig. 1 shows the relationship between MDD and the LZMT for the
three different PLC content while Fig. 2 shows the relationship between
the OMC and the LZMT also for the three different PLC content. From
Fig. 1, it can be seen that there was a corresponding increase in the MDD
for the three PLC contents as the percentage of the LZMT increased until
peak values were attained for the three different curves of the three PLC
contents. As illustrated in Fig. 1, the three curves for the three PLC
contents show similar trend. Interestingly, the combination of additives
(PLC and LZMT) that led to the increase in the MDD of the expansive soil
in all the curves shown in Fig. 1 was observed when a combination of
25% LZMT and 12% PLC were blended with the expansive soil.
Furthermore, as seen in Fig. 1, after the attainment of the peak MDD,
there was a gradual decrease in the MDD For the gradual increase in the
MDD until the attainment of the peak value; it could be attributed to the
higher specific gravity of the LZMT in comparison with that of the TBCS
as shown in Table 1. The high specific gravity of the additives imparted
significant strength on the expansive soil, which increase the MDD of the
soil. The increase in the MDD could also be attributed to the hydration
process experienced between the PLC and the moist soil-additive mix­
tures, which led to the formation of cementitious compounds (calcium
silicate hydrate (C–S–H), calcium aluminate hydrate (C-A-H), and
magnesium silicate hydrate (M-S-H)). The increased PLC in the soil-
additive mixtures obviously resulted in the sustainment of the hydra­
tion process, which in turn led to increased production of C–S–H, C–S-A-
H and M-S-H. The three cementitious compounds are known to be highly
stable and firm thus resulting in the increment observed in the MDD.
Similar trend was also observed by Ojuri et al. (2017) and Etim et al.
(2017). More importantly, the variations in the peak MDD values
observed in the three curves as shown in Fig. 1 may not be unconnected
with their PLC contents. The curve with the highest PLC content (12%)
was observed to have a much higher MDD than that of the other two
curves whose PLC contents are 8% and 4%. The soil-additive mixtures
with the highest PLC content produce more hydration products that led
to the highest MDD as depicted in Fig. 1. This clearly indicates that the
higher the PLC content, the higher the MDD. In the case of the reduction
in the MDD for the three curves after the attainment of their peak MDD
values when a combination of 25% LZMT and 12% PLC were blended
with the soil, this process could be attributed to the retarding effect of
the Pb2+ as explained in detailed in the concluding part of this section.
For a better appreciation and comprehension of the hydration
mechanism that led to the increase in MDD and the subsequent reduc­
tion in the MDD after the attainment of its peak value when a combi­
nation of 25% LZMT and 12% PLC were blended with the TBCS, the
following explanation will suffice. The increment in the MDD of the
expansive soil could be explicated in terms of the early hydration re­
action and solidification experienced between the expansive soil/LZMT
and the PLC. The early hydration occurred when the PLC came in con­
tact with water. The compounds of PLC widely known to be responsible
for hydration are dicalcium silicate, (β-Ca2SiO4 or C2S or 2CaO.SiO2),
tricalcium silicate, (Ca3SiO5 or C3S or 3CaO.SiO2), tricalcium aluminate
(Ca3Al2O6 or C3A or 3CaO.Al2O3) and tetracalcium alumnoferrite
(Ca4AlnFe2-nO7 or C4AF). However, due to the insufficient curing time of
the expansive soil-LZMT-PLC mixture, only the C3S and C3A may have
been mobilized for the hydration process. Both compounds are respon­
sible for the early hydration and the eventual early strength gain of the
mixture that led to the increase in the MDD of the expansive soil-LZMT-
PLC mixture.
A.O. Odumade et al. Journal of Environmental Management 321 (2022) 115980

Table 4
Elemental constituents of the LZMT, natural TBCS and stabilized TBCS.
Element Number Element Symbol Element Name LZMT TBCS Stabilized TBCS

Atomic Conc. Weight Conc. Atomic Conc. Weight Conc. Atomic Conc. Weight Conc.

14 Si Silicon 49.38 41.08 47.96 39.80 38.32 44.38

26 Fe Iron 9.91 16.40 16.76 27.66 3.21 6.28
13 Al Aluminium 20.79 16.62 22.05 17.58 17.6 6.98
19 K Potassium 8.25 9.55 3.44 3.97 0.61 0.78
20 Ca Calcium 3.27 3.89 2.76 3.27 32.93 35.07
22 Ti Titanium 1.53 2.17 1.84 2.60 0.6 0.81
17 Cl Chlorine 0.82 0.86 1.86 1.95 0.11 0.07
16 S Sulfur 1.06 1.01 0.74 0.70 1.79 1.63
15 P Phosphorus 0.71 0.65 0.70 0.64 0.48 0.42
12 Mg Magnesium 1.64 1.18 0.90 0.64 2.11 0.76
11 Na Sodium 1.12 0.77 0.90 0.61 0.17 0.11
82 Pb Lead 0.53 3.22 0.09 0.57 0.43 0.23
30 Zn Zinc 0.42 0.81 0.00 0.00 0.76 0.79
47 Ag Silver 0.56 1.80 0.00 0.00 0.88 1.69

The processes involved in the hydration of the C3A and C3S in the
expansive soil-LZMT-PLC mixture can be elucidated. The hydration
process of C3A, which is faster than that of the C3S, is the first to occur in
the mixture. The C3A undergoes a rapid exothermic reaction with water
molecules and the dissolved gypsum (CaSO4.2H2O) to produce a needle-
shaped crystal of calcium sulphoaluminate hydrate (Glasser et al.,
1999). The gypsum is a compound that is usually added during the
production of PLC to prevent flash set. Furthermore, the produced cal­
cium sulphoaluminate hydrate, which is also known as AFt-sulphate or
ettringite (Equation (14)), forms a membrane that coats the expansive
soil, LZMT and C3A grains. The membrane is also known to impede ions
diffusions from the solution of C3A that are yet to react with water (Chen
et al., 2009; Yousuf and Mollah, 1995). Nevertheless, the membrane
continuously gets ruptures, albeit slowly, and fresh reaction of the
coating continues until the sulphate and calcium ions become attenu­
ated. Subsequently, a stage is reached when the production of ettringite
is no longer favoured. At this stage, the ettringite gradually transforms
and precipitates into a similar compound known as AFm-sulphate or
calcium monosulphoaluminate (Equation (15)) that bonds the LZMT
and the expansive soil to increase the MDD of the expansive soil (Chen
et al., 2009; Taylor, 1971, 1997).
C3A + CaSO4.2H2O + 26H→C3A.3CaSO4.32H2O (ettringite) (14)
C3A + CaSO4.2H2O + 10H→C3ACaSO4.10H2O (calcium mono­
sulphoaluminate) (15)
In the case of the hydration of C3S that may have contributed to the
increase in the MDD of the expansive soil-LZMT-PLC mixture, two major
compounds namely, Portlandite (Ca(OH)2) and calcium silicate hydrate
gel (C–S–H) (Equation (16)) are produced when it comes in contact with
water (Shetty, 1982; Yousuf and Mollah, 1995; Taylor, 1986; Skalny and
Young, 1980). The produced C–S–H gel, which acts as a membrane that
envelopes the expansive soil, LZMT and C3S grains, allows water mol­
ecules to flow inward, and the silicate and Ca2+ ions to flow outward as a
result of the osmotic potential difference on either side of the membrane
(Yousuf and Mollah, 1995). Occasionally, the membrane ruptures and
gradually re-forms itself by extruding the concentrated silicate solution
in it (Chen et al., 2009; Yousuf and Mollah, 1995). This causes an
increased formation of the Portlandite, which subsequently accumulates
on the membrane fluid side, thus, effectively filling up the cavities in
between the grains. This phenomenon causes the additional increase
experienced in the MDD of the mixture.
2(3CaO.SiO2) + 6H2O →3CaO. 2SiO2. 3H2O + 3Ca(OH)2 (16)
Equation (16) can be expressed as
2C3S + 6H→C3S2H3 (C–S–H gel) + 3Ca(OH)2 (17)
Remarkably, aside the calcium-based compounds whose hydration
process resulted in the formation of cementitious compounds; the
magnesia (MgO) present in the materials (Table 2) could also have
contributed to the increase in the MDD of the soil-additive mixtures. The
hydration of MgO also results in the formation of cementitious com­
pounds. The MgO reacts with the soil-additive mixtures to form brucite
(Mg(OH)2). The brucite in turn reacts with the amorphous silica present
in the soil and the LZMT to produce the earlier mentioned cementitious
compound, MgO–SIO2–H2O (M-S-H) that also increased the MDD of the
soil-additive mixtures. Detailed explanation of the hydration mechanism
of MgO can be found in the literature (Li et al., 2014, 2017, 2018;
Vandeperre et al., 2008; Zhang et al., 2014). Finally, for the reduction
observed in the MDD (Fig. 1) of the expansive soil-LZMT-PLC mixture
after attaining its peak value can be explained in terms of the retarda­
tion/acceleration effect of LZMT on the hydration of the PLC. Generally,
heavy metals behave differently during the hydration of cement com­
pounds. Some heavy metals accelerate the hydration of cement com­
pounds such as C3S while others retard their hydration (Hills et al.,
1994; Smith et al., 1997; Tashiro et al., 1979). Pb2+ is a typical example
of heavy metal that accelerates the hydration of C3S while Zn2+ retards
its hydration (Chen et al., 2007). The Pb2+ found in the solution of the
LZMT in the mixture may have contributed to the rapid increase in the
hydration of C3S that led to the early production of the C–S–H and Ca
(OH)2 that causes the rise in the MDD. However, whilst the Pb2+ was
accelerating the hydration of C3S, the Zn2+ was retarding it. Eventually,
the effect of the Zn2+ dominated that of the Pb2+ in the hydration pro­
cess. The domination of the effect of Zn2+ over Pb2+ could be attributed
to its ability to readily form calcium zincates precipitate (CaZ­
n2(OH)6.2H2O) (Chen et al., 2007). The calcium zincates precipitate
coats the expansive soil and C3S grains thus, retarding the C3S hydration
process. Notably, as more fine particles of LZMT are added to the
mixture, the contribution of the Zn2+ became more pronounced, thus,
gradually reducing the MDD of expansive soil-LZMT-PLC (Fig. 1) and
increasing the water content needed for the reaction in the process as
shown in Fig. 2. Equations (16)–(17) show the chemical process involve
in the formation of the calcium zincates precipitate.
3.2. Regression analysis
Multiple regression models were developed using simple multiple
regression analysis to establish the relationship between the additives
(LZMT and PLC) used in this study and the compaction characteristics of
the modified expansive soil. The compaction characteristics, which were
the MDD and OMC, were the output variables and the additives were the
input or independent variables of the regression models. The models
developed for the MDD and OMC are presented in Equations (18) and
(19) respectively. Furthermore, the analysis of the developed models
performed to validate its prediction accuracy using a statistical metric,

7
A.O. Odumade et al. Journal of Environmental Management 321 (2022) 115980

Table 5
Analysis of Variance result.
Property Variation source df F-value Fcrit-value P-value

MDD PLC 2 72.234 4.1028 0.000001

LZMT 5 57.809 3.3258 0.0000005
OMC PLC 2 37.118 4.1028 0.0000236
LZMT 5 166.27 3.3258 0.00000000274

the adjusted R2 value, revealed that the adjusted R2 value was 98.96%
for the MDD while it was 96.74% for the OMC. These very high adjusted
R2 values for both the MDD and the OMC of the LZMT-PLC modified
expansive models suggest that they have good prediction and general­
ization ability.
MDD = 1.534 + 0.00512LZMT + 0.006PLC (18)

OMC = 23.932 − 0.297LZMT − 0.2302PLC (19) Fig. 3. FTIR spectra of TBCS.

3.3. Analysis of variance (ANOVA)

Analysis of variance (ANOVA) was performed on the developed

models to ascertain the statistical significance of the additives used for
their development. The results of the ANOVA are displayed in Table 5.
From Table 5, it can be seen that the effects of both additives (LZMT and
PLC) on the MDD model are statistically significant. The LZMT gave an
F-value of 57.809 and Fcrit–value of 3.3258, which indicates that the
F–value > Fcrit–value. Similarly, it can also be seen from Table 5 that the
PLC is statistically significant as the F-value and Fcrit–value were 72.234
and 4.1028 respectively, which also indicate that the F–value >
Fcrit–value. More importantly, the P-values for both the LZMT and the
PLC, which were estimated respectively as 0.0000005 and 0.000001,
were far less than the critical P-value of 0.05. This clearly reveals that
they are statistically significant in the development of the MDD model.
In a related analysis, the result of the ANOVA presented in Table 5
also indicates that both additives (LZMT and PLC) are statistically sig­
Fig. 4. FTIR spectra of LZMT.
nificant or have a substantial contribution in the developed OMC model.
The LZMT gave an F-value and an Fcrit–value of 166.27 and 3.3258
respectively, which indicates that the F–value > Fcrit–value. In the same
vein, the PLC, as depicted in Table 5, is also found to be statistically
significant as its F-value and Fcrit–value were 37.12 and 4.1028
respectively, which indicates also that the F–value > Fcrit–value. More­
over, the P-values for both the LZMT and the PLC, which were estimated
respectively as 0.00000000274 and 0.0000236, were less than the
critical P-value of 0.05. This clearly lends credence to their statistical
significance in the development of the MDD model.

3.4. Microstructural analysis

The microstructural analyses (FTIR and SEM) in this study were

carried out using the optimum mix ratio, which was obtained from the
UCS result as a combination of 25% LZMT and 12% PLC. The 28 days
UCS result of the optimum mix ratio was obtained as 675.12 kN/m2
(Table 3). This UCS value, according to the Federal Ministry of Works
highway design manual Part 1 (2013), exceeds the minimum value of
500 kN/m2 that can be used in the design of subgrade for light traffic
roads. This implies that the UCS obtained for the TBCS stabilized with
the optimum mix ratio (25% LZMT and 12% PLC) exceeded that of the Fig. 5. FTIR spectra of the TBCS stabilized with an optimum mix (25% LZMT –
minimum value (500 kN/m2) stipulated by the Federal Ministry of 12% PLC).
Works highway design manual part 1 (2013) by about 35%. It also in­
dicates clearly that the stabilized soil can adequately serve as subgrade material.
material in pavement construction. However, based on the US Army
Technical manual No. 5-822-14/Air Force AFJMAN 32–11019 (Gordon 3.4.1. Effect of additives on the FTIR of TBCS
et al., 1994; Edeh et al., 2022), the stabilized TBCS cannot be used as The results of the FTIR test on the TBCS and LZMT are shown in
subbase or base material because its UCS fell short of the minimum value Figs. 3 and 4 respectively. From Fig. 3, the bond around 1650 cm− 1
stated in the US Army Technical manual No. 5-822-14/Air Force AFJ­ indicates the formation of MgCO3. It also indicates the pozzolanic
MAN 32–11019 which is 1720 kN/m2. It can only be used as subgrade

8
A.O. Odumade et al. Journal of Environmental Management 321 (2022) 115980

Fig. 6. EDX spectra of TBCS.

Fig. 7. EDX spectra LZMT.

Fig. 8. EDX spectra of the TBCS stabilized with an optimum mix (25%LZMT-12%PLC).

9
A.O. Odumade et al. Journal of Environmental Management 321 (2022) 115980

Fig. 9. SEM image of natural TBCS.

character of the black cotton soil in the presence of Si–O and Al–O
tension bond with the bonds around 1000 cm− 1 wavenumber, while the
bonds around 900 cm− 1 correspond to Si–O–Si bonds. Fig. 4 indicates
the pozzolanic character of the LZMT in the presence of Si–O and Al–O
tension bond; with the bonds around 1000 cm− 1 wavenumber. The bond
around 1500 cm− 1 indicates the formation of MgCO3 (Zhang et al.,
2016); while the bonds around 800 cm− 1 correspond to Si–O–Si bonds.
The presence of CaO or Ca(OH)2 is indicated by the bonds around 3620
cm− 1 which activates SiO2 and Al2O3 thereby forming the C–S–H gel
structure.
The TBCS was treated with the optimal mix based on the strength
properties for sub – base layers, and the matrix was tested for micro­
structural analysis using FTIR test. The result is presented in Fig. 5. The
TBCS – LZMT – PLC matrix is observed to contain more hydrated silicate
due to the presence of the additives especially the cement content
(Palomo and Fuente, 2003). The results show five absorbances which
peak at 3568.9 cm− 1 indicating free hydroxyl representing the presence
of CaO or Ca(OH)2, the presence of this pozzolanic constituent is so
prominent by the presence of the several peaks around the bond at 3500
cm− 1. The bond around 2000 cm− 1, which peaks at 1964.3 cm− 1 is also
observed to have several peaks, and this indicates the formation of
MgCO3 representing the alkene group. The absorbances around bond
1000 cm− 1 indicate the presence of Si–O and Al–O tension bonds, rep­
resenting the alkyl amine and alkyl ketone (Palomo and Fuente, 2003).
From the result, the matrix is observed to be in an excited state indi­
cating a high presence of CaO and SiO2, thereby producing a better
cementitious compound.

Fig. 10. SEM image of LZMT.

10
A.O. Odumade et al.
Fig. 11. SEM image of TBCS stabilized with an optimum mix ratio.
3.4.2. Scanning electron microscopic (SEM) analysis for the natural TBCS,
LZMT and stabilized TBCS
Generally, elemental constituent analysis is used to depict each
element of a material in terms of its atomic concentration and its con­
centration by weight. Fig. 6 shows the EDX spectra of the TBCS while
that of the LZMT and the TBCS stabilized with the optimum mix ratio are
displayed in Figs. 7 and 8 respectively. These elements are also pre­
sented lucidly in Table 4 for both the TBCS and LZMT. As shown
respectively in Figs. 6 and 7, the EDX spectra of the TBCS and LZMT
indicate the presence of elements in the samples.
In addition, Figs. 6 and 7 also show that silicon is the most abundant
element in both TBCS and LZMT followed by aluminium and iron. Major
elements found to be present are Si and Al, while minor presence of
elements such as Ca, Al, Mg, Fe, Na, K, Ag etc. are observed. From
Table 4, the ratios of Ca/Si and Ca/Al respectively for the TBCS are 0.06
and 0.125, which suggest that the soil exhibit poor strength and stiffness
Fig. 12. Grayscale image of natural TBCS.
11
Journal of Environmental Management 321 (2022) 115980
behaviour which is typical of expansive soil (Ikeagwuani and Nwonu,
2019). The very high content of silicon in the soil in comparison to the
low calcium content is evident with the low Ca/Si ratio which contrib­
utes to the poor binding ability of the soil. In a related development, the
EDX spectra of the TBCS stabilized with the optimum mix ratio in Fig. 8
showed high peak values for Ca when compared with that of the natural
TBCS. Similarly, from Table 4, the ratios of the Ca/Si and Ca/Al were
observed to increase to 0.86 and 1.87 respectively. These two values for
the stabilized TBCS are higher than the corresponding values observed
for the natural TBCS. This clearly indicates the production of cementi­
tious compounds in the sample of TBCS stabilized with the optimum mix
ratio (25% LZMT – 12% PLC). The produced cementitious compounds,
which are essentially those of C-A-S-H, C–S–H and M-S-H gel, suggests
the existence of cation exchange activity during the occurrence of the
pozzolanic reaction between the TBCS and the optimum mix ratio. This
is evident in the stiffened behaviour of the macrostructure for the
A.O. Odumade et al.
Fig. 13. Grayscale image of TBCS stabilized with an optimum mix ratio.
Fig. 14. Determination of fractal dimension using GEOBOX COUNT.
stabilized TBCS. This finding is in agreement with the study executed by
Nwonu & Ikeagwuani (Nwonu and Ikeagwuani, 2021) and Muhammad
et al. (2018). Lastly, in another development, Figs. 9 and 10 show the
SEM images of both TBCS and LZMT respectively. While the TBCS im­
agery shows unbounded individual grains, the SEM image of LZMT show
flocculates of tailings with reduced porosity.
3.5. Pore characteristics
Fig. 11 shows the SEM image of the stabilized mix which indicates a
matrix with a stronger aggregation and bond. Figs. 12 and 13 show the
binary image of the grayscale SEM image of the TBCS and the stabilized
expansive soil respectively generated with the adaptive segmentation
technique described in Section 2.2.3 while Fig. 14 shows the GEOBOX
COUNT image used for the determination of the fractal dimension. The
fractal dimension as shown in Fig. 14 is 1.8745 ± 0.23746. This implies
that the fractal dimension could range from 1.64 to 2.11. The value 2.11
was adopted in this study as the fractal dimension to evaluate the pore
12
Journal of Environmental Management 321 (2022) 115980
structure characteristics. Substituting the fractal dimension as 2.11 into
Equations (12) and (13), the values of the tortuosity and porosity were
obtained respectively as 1.468 and 34.6%. Furthermore, for the esti­
mation of the permeability, Equation (10) was used. The value deter­
mined for the permeability was 5.345 × 103 nm2. The values obtained
for the pore structure characteristics, especially the porosity clearly
suggest that the stabilized expansive soil could have a slight reduction in
its strength properties. It has been that demonstrated by Chen et al.
(2020) that there is an inverse relationship between porosity and
compressive strength of a material.
4. Conclusion
The influence of the combination of LZMT and PLC on the compac­
tion and microstructural analysis of an expansive soil has been evaluated
in this study. Based on the compaction tests and the microstructural
analysis conducted in the study, the following conclusions can be drawn:
A.O. Odumade et al.
1. The use of LZMT and PLC as additives improved the microstructural
arrangement and influenced the chemical configuration of the
matrix.
2. The stabilization of the TBCS with LZMT and PLC additives led to an
increase in MDD and a decrease in OMC of the TBCS.
3. The mix ratio which led to optimal performance of the expansive soil
was obtained as 20% LZMT and 12% PLC. The optimum mix gave an
improved microstructural composition based on the microstructural
tests conducted, establishing that the optimum matrix is in an excited
state, thus forming compounds that have better binding properties.
4. The LZMT and PLC mix is seen to contribute immensely to the
chemistry of the matrix as seen in the FTIR results of the optimum
mixes. The FTIR test result indicated the presence of more com­
pounds that aid the performance of the soil, establishing the for­
mation of C–S – H gel structure and producing more hydrated
silicate.
5. The pore structure characteristics of the stabilized expansive soil
which were obtained using a combination of image segmentation
technique and fractal geometry indicate the possibility of a slight
reduction in the strength of the stabilized soil due to its high level of
porosity.
Credit author statement
Odumade, A.O: Conceptualization, Methodology, Software, Data
curation, Writing – original draft, Resources, Formal analysis. Okafor,
F.O: Visualization, Supervision, Resources. Ikeagwuani, C.C: Software,
Validation, Writing- Reviewing and Editing, Resources, Formal analysis.
Declaration of competing interest
The authors declare that they have no known competing financial
interests or personal relationships that could have appeared to influence
the work reported in this paper.
Data availability
Data will be made available on request.
Acknowledgements
The authors highly commend and appreciate the immeasurable
contribution of the anonymous reviewers of this paper whose
constructive reviews significantly enhance its clarity and technical
content.
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