Engineering Geology 318 (2023) 107101

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Engineering Geology
journal homepage: www.elsevier.com/locate/enggeo

Microstructural evolution of saturated normally consolidated kaolinite clay

under thermal cycles
Seyed Morteza Zeinali, Sherif L. Abdelaziz *
The Charles E. Via, Jr., Department of Civil and Environmental Engineering, Virginia Tech, Blacksburg, VA, USA

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

Keywords: This study aims to quantify the microstructural evolution of saturated clay during one thermal cycle. For this
Thermal behavior of soils purpose, five saturated normally consolidated kaolinite clay triaxial specimens were consolidated under the same
Microstructure analysis conditions. One specimen was subjected to a mechanical consolidation only; while the other four specimens were
Mercury intrusion porosiemtry
subjected to different thermal paths: freezing (F), freezing-thawing (FT), freezing-thawing-heating (FTH), and
Specific surface area
SEM
freezing-thawing-heating-cooling (FTHC). After completing the mechanical and thermal stages, thin disks were
cut from the bottom of each specimen. The microstructures of these disks were preserved using flash freezing and
freeze-drying. The evolutions of the microstructure of the specimens during the thermal cycle was assessed using
mercury intrusion porosimetry, gas adsorption methods, and processing of scanning electron microscopy (SEM)
images. The results show that (1) freezing increased the modal throat size and the specific surface area (SSA); (2)
freezing-thawing decreased both modal throat and pore sizes, while the SSA recovered to its initial value; (3)
freezing-thawing-heating reduced the pore and throat sizes and SSA even further; and (4) freezing-thawing-
heating-cooling caused permanent reduction in SSA and throat and pore size distributions. Finally, the shape
of the pores became more circular after temperature changes, while the number of pores increased during the
thermal cycle with the highest number corresponding to the end of heating (i.e., the third stage in the thermal
cycle).

1. Introduction Ghasemi-Fare, 2019; Tamizdoust and Ghasemi-Fare, 2020),which in­

Temperature rise as a consequence of climate change growingly
exposes more frozen grounds to thawing. It also affects the freeze-
thawing states of soils by increasing the number of warmer days and
decreasing the number of cold ones (Peng et al., 2017; Wang et al.,
2020a). The loss of shear strength of soils after thawing (Broms and Yao,
1964; Han et al., 2018; Steiner et al., 2018), along with the increased
temporal extent of the thawed state of the ground, may lead to several
disastrous events such as thaw-induced landslides (Niu et al., 2016;
Morino et al., 2021). Moreover, in the past decades, the rising urge for
the utilization of sustainable energy sources to reduce the negative ef­
fects of fossil fuels has triggered many geotechnical engineering appli­
cations to exploit geothermal energy. These applications, such as energy
piles, subject soils to heating-cooling cycles (Abdelaziz et al., 2011;
McCartney et al., 2011; Olgun et al., 2012; Coccia et al., 2013; Ghasemi-
Fare and Basu, 2013; Laloui and Di Donna, 2013; Abdelaziz et al., 2014;
Ng et al., 2014; Goode and McCartney, 2015; Loria et al., 2015; Abde­
laziz and Ozudogru, 2016; Loria and Laloui, 2017; Tamizdoust and
creases the hydraulic conductivity of the ground hosting borehole heat
exchangers and induce permanent volume reduction in the soil (Dalla
Santa et al., 2016a, 2016b; Dalla Santa et al., 2019). Therefore, a thor­
ough understanding of the response of soils to different temperature
cycles for the purpose of engineering the unfavored thermal behavior of
grounds and increasing the efficiency of geothermal applications is
crucial.
While freezing temperatures in thermo-active geostructures are
generally avoided to ensure the geostructure and the surrounding soils
do not suffer from the freezing-thawing effects (Abdelaziz, 2016), faulty
designs or interrupted operation of these thermal elements may result in
undesired freezing-heating cycles in the soils. Furthermore, freezing-
heating cycles are common in soils surrounding closed-loop vertical
heat exchangers. These cycles may impact the thermal performance of
the heat exchangers due to changes in the pore structure, void ratio,
thermal properties, and flow of water around these elements.
Geothermal heat exchangers that experience freezing-heating cycles
suffer from differential thermal expansion and contraction of the backfill

* Corresponding author.
E-mail addresses: smzeinali@vt.edu (S.M. Zeinali), saziz@vt.edu (S.L. Abdelaziz).

https://doi.org/10.1016/j.enggeo.2023.107101
Received 30 June 2022; Received in revised form 8 December 2022; Accepted 27 March 2023
Available online 29 March 2023
0013-7952/© 2023 Elsevier B.V. All rights reserved.
S.M. Zeinali and S.L. Abdelaziz
and soil materials; these differences may result in gap development at
the interface between the backfill material and the surrounding soil or a
break in the backfill material. These discontinuities compromise the
thermal efficiency of the geothermal heat exchangers.
The macroscale thermal response of clays has been widely studied in
the literature. During the freezing, negative pore pressure develops
within the sample that consequently increasing the effective stress
(Morgenstern and Nixon, 1971; Chamberlain and Blouin, 1977; Cham­
berlain, 1981). Thawing, however, generates excess positive pore water
pressures. The dissipation of excess pore pressure induces a permanent
reduction in void ratio after a freeze and thaw cycle, which is known as
thawing-induced consolidation (Morgenstern and Nixon, 1971; Lesage,
2008; Yao et al., 2017). Despite the decrease in void ratio at the end of
thawing, an increase in the hydraulic conductivity of soils has been re­
ported by many studies, which attributed to permanent macro- and
micro-structural damage (Benoit and Voorhees, 1990; Chamberlain
et al., 1990; Othman and Benson, 1993; Dalla Santa et al., 2019).
Moreover, normally consolidated clays and lightly over-consolidated
clays contract during temperature increment as they experience a
decrease in void ratio. As for heavily over-consolidated clays (with OCR
more than ~4), expansion during drained heating is expected (Baldi
et al., 1988; Cekerevac and Laloui, 2004; Abuel-Naga et al., 2007a;
Coccia and McCartney, 2016). Furthermore, during cooling after heat­
ing, normally consolidated clays dilate, experiencing a permanent
contraction at the end of the heating-cooling cycle (Abuel-Naga et al.,
2007b; Bai et al., 2014; Samarakoon and McCartney, 2020). However,
the magnitude of the thermally induced permanent contraction is also
dependent to stress history (Baldi et al., 1988; Abuel-Naga et al., 2007a).
Lightly overconsolidated clays exhibit thermo-elastic behavior or
negligible irreversible contraction with a heating and cooling cycle. In
contrast, heavily over-consolidated clays contract during cooling, with a
pronounced permanent expansion at the end of cooling (Abuel-Naga
et al., 2007a).
Predicting and engineering the adverse behavior of soils under
various temperatures mandate comprehensive insights into the alter­
ations caused by the changes in the temperature of the ground. How­
ever, the thermally-induced changes of soil behavior are not fully
appreciated without perceiving the microstructural alterations caused
by thermal loads and their corresponding micro-scale underlying me­
chanics. There exist several studies on how extreme temperatures from
temperatures below freezing to elevated temperatures or thermal cycles
such as freezing-thawing (Chamberlain et al., 1990; Othman and Ben­
son, 1993; Zhang and Cui, 2018; Dalla Santa et al., 2019; Wang et al.,
2020b; Zeinali and Abdelaziz, 2020a) or heating-cooling (Jaradat and
Abdelaziz, 2020; Zeinali and Abdelaziz, 2020b) alter the soil structure.
These studies showed that the soils' microstructure react to the thermal
loads by (1) changing the pore size distribution (Darbari et al., 2017;
Othman and Benson, 1993; Zeinali and Abdelaziz, 2022; Houhou et al.,
2021), (2) particle reorientation (Jaradat et al., 2017; Abdelaziz et al.,
2020) and (3) interparticle forces (Jaradat and Abdelaziz, 2020).
Despite the discussed efforts to comprehend the thermal response of the
soils in the microscale, how experiencing one extreme temperature may
affect the expected response at the other extreme and the link between
micro-, and macro-scale behaviors are not investigated thoroughly. The
study of the microstructural response of soils to various thermal or
mechanical loadings and how it is reflected in macroscale behavior fa­
cilitates the development of more robust constitutive models. Micro-
scale study of the response of soils to thermo-mechanical loading does
not only reveal the underlying mechanics of macro-scale behavior of
soils, but it also provides more insightful engineering approaches to
engineer the ground against unfavorable responses under various
thermo-mechanical conditions. For example, the efficiency of geo­
materials engineered by using additives such as cement (Tebaldi et al.,
2016; Arasan et al., 2017) to compensate for the strength loss due to
thawing is determined by the physio and chemical interactions of the
soil with the additive. The frontline of these interactions are the pores of
2
Engineering Geology 318 (2023) 107101
the soil medium. Transferring the knowledge of the changes applied to
the microstructure due to thermal loads into geotechnical applications
and problems facilitates upgrading the performance and efficiency of
these engineered geomaterials. For this purpose, this study aims to
broaden the understanding of the micro-scale response of saturated clay
to temperature changes. Therefore, the evolution of pore size distribu­
tion, specific surface area, and volumetric strains under a full thermal
cycle of freezing, thawing, heating, and cooling are assessed in this
study.
2. Materials and methods
2.1. Thermo-mechanical triaxial system
In this study, a thermo-hydro-mechanical triaxial cell manufactured
by Global Digital Systems (GDS) was used. This triaxial system has a
well-insulated cell and is capable of changing the temperature of the
specimens between − 20 ◦ C to 70 ◦ C. An oil-based cell fluid was used,
which allows the freezing of soil specimens without freezing the cell
fluid. The temperature of the triaxial cell was controlled by circulating
oil in an internal coil. The temperature was applied isotropically and
measured using a thermistor installed close to the specimen but in the
cell fluid. Thus, a thermal calibration was performed following the steps
adopted by Jaradat and Abdelaziz (2019), correlating the temperature
of the cell fluid to the temperature at the center of a sacrificial specimen.
The results of this calibration were used to target the desired specimen
temperatures in this study.
The volume changes experienced by the considered soil specimens
were measured using two systems: local Linear Variable Differential
Transformer (LVDTs) installed directly on the specimens and the volume
changes of the backpressure pump. The former system consists of two
local LVDTs attached to the soil specimen; one records the axial dis­
placements, while the other records the radial displacement. This system
is critical, especially during the freezing stage, since the water in the
drainage lines freezes, preventing the measurements of volume changes
using the backpressure pump (i.e., the second system). Moreover, during
the thawing stage, the ice in drainage lines changed phase before the soil
specimen; consequently, the volume change of the back volume pump
does not reflect the actual volume change of the specimen and also in­
cludes the volume drained out of the drainage system. On the other
hand, the volume of the backpressure pump is considered more accurate
at elevated temperatures since the glue connecting the local LVDTs to
the latex membrane experiences some volume changes, compromising
the readings of the local LVDTs. Thus, volumetric strains during freezing
and thawing stages were measured using the local LVDTs, while the
volume of the backpressure pump was used to measure the volumetric
strains during the isotropic consolidation, heating, and cooling stages.
Finally, the effects of the temperature changes on the different compo­
nents of the triaxial system, including the local LVDTs, and volume of
the backpressure pump, were calibrated, following the (Jaradat and
Abdelaziz, 2019) procedure, for the different mechanical and thermal
loadings considered in this study.
2.2. Selected clay, specimen preparation and thermal paths
Edgar Plastic Kaolin (EPK) was used to prepare bulk clay blocks. The
EPK (purchased from Edgar, FL) has >96% Kaolinite mineral with a
plastic limit of 32% and a liquid limit of 67%. It, thus, classifies as high
plasticity clay (CH) according to the Unified Soil Classification System
(USCS) (Palomino et al., 2008; Darbari et al., 2017). This commercial
clay consists of >96% Kaolinite minerals, unlike a natural soil which
typically contains multiple percentages of various minerals. Working
with a clay as close as possible to be purely consistent of one mineral
simplifies the analysis since it allows us to eliminate the effect of
different thermal expansion coefficients in the soil sample. To prepare
bulk clay blocks, the clay powder was first mixed with deionized water
S.M. Zeinali and S.L. Abdelaziz Engineering Geology 318 (2023) 107101

at 150% of the liquid limit. Then, the uniform slurry was poured into a
mold and consolidated solely under the weight of a custom-made
loading cap for 24 h to minimize piping. After 24 h, the slurry was
subjected to 1-D incremental loading up to vertical stress of 100 kPa.
Once the consolidation stage was completed, the bulk clay block was
extracted from the mold and preserved in plastic wrap in a temperature-
controlled humidity room.
Five cylindrical triaxial specimens, with heights of ~82 mm and
diameters of ~50 mm, were trimmed out of the bulk clay blocks. All
specimens were saturated using the backpressure method to a Skemp­
ton's B-value of >95%. All specimens were then consolidated under
isotropic stress of 400 kPa at the selected reference temperature (20 ±
0.03 ◦ C). Providing that the clay bulks were consolidated under 100 kPa,
the consolidation stress of 400 kPa ensures that these clay specimens are
normally consolidated. The first specimen (Specimen ISO in Table 1)
was extracted out of the triaxial cell upon the completion of the
consolidation stage, as it was used as a reference in the comparison
against the other specimens.
Each of these other four specimens was subjected to a thermal path,
applied isotopically, representing the end of one stage of a full freezing-
thawing-heating-cooling cycle. In other words, one specimen was sub­
jected to a freezing (F) path, the second specimen was subjected to a
freezing-thawing (FT) path, the third specimen was subjected to a
freezing-thawing-heating (FTH) path, and the last specimen was sub­
Fig. 1. The temperature versus time for sample FTHC, with average rate of
jected to the full freezing-thawing-heating cooling (FTHC) path. Table 1
temperature change at each stage in centigrade per minute (CPM).
lists the temperature changes, dimensions, and initial saturated void
ratios, along with the void ratio at the end of mechanical consolidation
and thermal loads for each of the considered specimens. Mechanical and separating the effect of the temperature from the thermally-induced
water flow. Then, the disks were swiftly submerged in liquid nitrogen
thermal stages were performed under single drainage conditions by
connecting the backpressure pump to the top of the sample and to preserve their microstructure (Sasanian and Newson, 2013); a subli­
mation of pore water rapidly frozen by liquid nitrogen at its melting
measuring the pore water pressure at the bottom where the drainage is
closed. The mutual thermal stages between the specimens in Table 1 point minimizes the microstructural damage caused by drying tech­
niques (Mitchell and Soga, 2005). The disks were then dried using the
were performed for the same duration of 10 h, ensuring comparable
mechanical and thermal states for all specimens. For demonstration, the freeze-drying method, which dries the samples through a direct phase
change of the pore ice from solid to vapor. This process prohibits the ice
cell fluid temperature against time is presented in Fig. 1 for sample
experiencing freezing, thawing, heating, and cooling (FTHC). from thawing and consequently avoids wetting of the pores and mini­
mizes the disturbance to the microstructure (Mitchell and Soga, 2005).
After freeze-drying the disks, they were placed in a desiccator under a
2.3. Post thermal cycles microstructural samples vacuum to prohibit them from adsorbing ambient moisture until their
microstructure was characterized. In this process, which is in accor­
After the completion of the thermo-mechanical loading on each dance with ASTM D4404–18, the pore water freezes virtually instanta­
triaxial specimen, specimens were extracted out of the triaxial cell. Thin neously, the crystallization of water is prevented, and the resulting pore
disks (~5 mm) were then cut from the bottom of the specimen, i.e., near ice is amorphous (Galle, 2001). Consequently, no large ice crystals form
the undrained boundary. The lower portion of the specimens was chosen and damage the microstructure. While there are several processes of
for microstructural investigation because the closed external drainage at microstructural preservations (e.g. air drying, oven drying, freeze-
the bottom of the specimen minimizes the effect of unloading on the drying and etc.), studies comparing these methods showcased the min­
microstructure during the extraction of the specimen (Pedrotti and imal damage to the microstructure imposed by flash freezing in liquid
Tarantino, 2018). Furthermore, the bottom of all used specimens Nitrogen and subsequent freeze drying (Gillott, 1970; Zimmie and
experienced the same conditions throughout the entire testing program Almaleh, 1976; Garcia-Bengochea et al., 1979; Tovey and Wong, 1980;
(i.e., undrained). This condition was indeed selected to minimize the Galle, 2001).
effect of the boundary condition by eliminating water flow out of this
location under large gradients, which would have happened if the
drained condition had been applied at the bottom. This allows

Table 1
Specimens' characteristics and thermal paths.
Specimen name Thermal path Diameter Height Void ratio after Void ratio after Void ratio after final Thermally-induced
(◦ C) (mm) (mm) saturation, e consolidation, ec thermal path, ef volumetric strain, εth (%)

Isothermal Consolidation 20 47.96 82.80 1.15 0.91 – –

(ISO)
Freezing (F) 20 → (− 15) 48.32 82.85 1.17 0.93 1.12 − 9.84
Freezing-Thawing (FT) 20 → (− 15) → 48.37 82.51 1.16 0.92 0.87 2.60
20
Freezing-Thawing-Heating 20 → (− 15) → 47.79 82.00 1.13 0.89 0.77 6.34
(FTH) 60
Freezing-Thawing- 20 → (− 15) → 48.43 82.33 1.16 0.93 0.78 7.78
Heating-Cooling (FTHC) 60 → 20

3
S.M. Zeinali and S.L. Abdelaziz
2.4. Specific surface area using nitrogen gas adsorption
For estimating the specific surface area (SSA), NOVAtouch LX4
surface area analyzer manufactured by Quantachrome Instruments was
used. First, samples with a total weight of ~0.2 g were cut out of the
freeze-dried disks. The pores within these samples were cleaned from
any possible dirt or absorbed moisture during sample preparation by
placing the samples into adsorption cells and degassing them under
vacuum at 100 ◦ C for 12 h. A degassing temperature of 100 ◦ C was
selected in accordance with a previous study on the effect of degassing
temperature on specific surface area measurements of Kaolinite clay
(Brooks, 1955). Brooks (1955) revealed that the specific surface area
measured for Kaolinite clay decreased from 7.2 m2/g to 6.8 m2/g, when
the degassing temperature changed from 25 ◦ C to 300 ◦ C. Therefore, the
selected degassing temperature has minimal impact on measured values
of specific surface area. The adsorption cells were transferred into the
analysis chamber, and then Nitrogen adsorption and desorption mea­
surements were conducted at − 196 ◦ C. Finally, the SSA was estimated
using Brunauer-Emmet-Teller (BET) method, which is an extension to
Langmuir's unimolecular layer theory (Brunauer et al., 1938).
Multiple N2-sorption experiments were conducted on different
comparable samples obtained from different locations of the disks, and
the average values were calculated. However, the comparison of average
SSA was solidified by performing statistical analysis to estimate the
required number of experiments using Eq. (1). This equation was used,
assuming that the measured values of SSA follow a normal distribution.
However, this assumption was validated, as discussed later.
( )
Zα/2 σ 2
n= (1)
E
where n is the number of samples needed to achieve acceptable error (E)
in the estimation of the mean of the population with a standard devia­
tion of (σ ) at a confidence interval of (α), and Ζα/2 is the normal distri­
bution Z-score. This exercise showed that a total number of 16 SSA
measurements for each of the considered thermal paths yields an esti­
mation of the mean value with an error (E) of <1% with a significance
level (α) of 0.05. Furthermore, the statistical significance of the obtained
values of average SSA was tested by two-tail t-tests, as discussed later.
Fig. 2 shows the relative location of the 16 samples used for the SSA
measurements out of the disks obtained from the considered triaxial
specimens.
2.5. Mercury intrusion porosimetry (MIP)
The pore size distribution and total volume of the pores were
measured using an automated mercury intrusion porosimeter (MIP)
Fig. 2. Relative locations of the microscale samples used for SSA and MIP
measurements.
4
Engineering Geology 318 (2023) 107101
PoreMaster 60 manufactured by Quantachrome, following ASTM
D4404-18 (2018). MIP involves the intrusion and extrusion of mercury,
as a non-wetting liquid, into and out of the pores. The maximum
intrusion pressure was set to ~413,685 kPa and applied incrementally.
Once the maximum pressure was achieved, the mercury was unloaded
back to 0 kPa while measuring the extruded volume of mercury. MIP is
able to measure the pore size distribution for pores ranging from ~4 nm
up to few millimeters. The pore size distribution measurement started by
placing small samples with a total mass of ~0.95 ± 0.02 g into pene­
trometers; these MIP samples consisted of five of the 0.2 g samples used
for the SSA measurements, as shown in Fig. 2. The penetrometers were
then mounted inside the low-pressure chamber of the instrument, where
the samples were first subjected to a vacuum; this step is used to clean
the samples and the penetrometers from any physisorbed materials.
Then, low-pressure intrusion under a gradually increasing pressure up to
344.78 kPa was performed. Once this pressure was reached, the pressure
was reduced back to ambient then the penetrometers were transferred
into the high-pressure intrusion chamber, where mercury was pressur­
ized to the maximum capacity of the instrument (~413,685 kPa).
Finally, after unloading the samples to the ambient pressure, the
resulting total volume of intruded and extruded mercury was obtained.
Assuming a cylindrical pore and utilizing the capillary flow theory
(Washburn, 1921), the inverse relationship between the pressure and
pore radius can be expressed by Eq. (2).
2γm cosθm
r= (2)
P
where r is the pore radius, P is the intrusion or extrusion pressure, γ m is
the surface tension of mercury (0.48 J/m2), and θm is the contact angle
between mercury and soil particles (149◦ ). The inverse relation between
pore size (r) and intrusion pressure (P) suggests that the smaller the pore
radius is, the higher the pressure required for the non-wetting mercury
to intrude into that pore.
An increase in pressure (Δp) corresponds to a decrease in the pore
radius (r-Δr). The intruded volume of mercury accompanying Δp fills the
pores with effective radii ranging between r and r-Δr. Therefore, if dV is
the volume of pores in one gram of a sample and with radii ranging
between r and r-Δr, then dV can be given by Eq. (3).
dV = Dv (r)dr (3)
where Dv(r) is the pore size distribution function, defined as the pore
volume per unit interval of radius. Substituting the derivative of Eq. (2)
into Eq. (3), Dv(r) can be estimated using Eq. (4).
( )
p dV
Dv (r) = − (4)
r dp
Although there are various classifications of pore size, the classifi­
cation considered in this study is in accordance with the one introduced
by the International Union of Pure and Applied Chemistry (IUPAC),
which is applicable to all porous media (Everett and Koopal, 2001;
Thommes et al., 2015). The IUPAC groups the pores into micropores
(diameters <2 nm), mesopores (diameters from 2 nm to 50 nm), and
finally, macropores (diameters >50 nm). The preliminary measure­
ments of pore size distribution on the samples showed that the EPK clay
samples were mostly dominated by the latter pore sizes, i.e., macro­
pores. With this type of medium, the logarithmic radius distribution
function Dv(log r) is a more accurate representation of pore size distri­
bution (PSD) (Liu and Ostadhassan, 2019). This function is expressed by
Eq. (5).
dV rdV
Dv (logr) = = = rDv (r) (5)
dlogr dr
Combining Eqs. (4) and (5) yields Eq. (6).
S.M. Zeinali and S.L. Abdelaziz
dV
Dv (logr) = − (6)
dlogp
Since the change in volume is measured as a decreasing volume, the
negative sign can be eliminated. Eq. (6) represents a convenient way of
reducing the cumulative curve to the size distribution curves.
In a porous media, larger pores are connected via smaller pores;
these thinner connections are mostly referred to as “throats.” During the
mercury intrusion, the size of the throats governs the intrusion of mer­
cury into the inner pores. According to Eq. (2), the pressure required to
fill a thin throat is higher than that needed to fill a large pore. Thus,
mercury cannot fill the pores unless the pressure is high enough for
mercury to pass through the bounding throats. This phenomenon is re­
flected in the emergence of a clear and sharp inflation point in the
intrusion curve (Wardlaw et al., 1988; Zhou et al., 2010). Furthermore,
mercury withdraws from the porous medium as the pressure decreases
during the extrusion stage. Since the pores are of larger diameters than
the throats, the pressure at which mercury is retracted from a pore is
lower than that at which mercury clears the shielding throats. During
the process of mercury extraction, thus, the mercury in the large pores
“snap-off” the continuous retracting of mercury from the pores (Ward­
law et al., 1988; Giesche, 2006). This “snap-off” process entraps mercury
in the pores, which explains the inability to extrude all intruded mercury
out of the porous media. Accordingly, intrusion curves are mostly gov­
erned by the throats, while extrusion curves are controlled by the
shielded pores (Wardlaw et al., 1988; Zhou et al., 2010). Thus, the size
distributions obtained from intrusion and extrusion curves represent the
size distributions of the throats and the pores in the media, respectively.
On a final note, the statistical analysis of the required number of samples
for mercury intrusion porosimetry yielded an unpractical large value;
however, it is common practice to rely on a single sample for compar­
ative study (Giesche, 2006; Sasanian and Newson, 2013; Zhang and Cui,
2018).
2.6. Scanning electron microscope (SEM) imaging
Small samples with smooth surfaces parallel to the bedding plane
were glued to SEM sample holders using silver paint. Then, the samples
were coated with 20 nm of palladium and platinum using a Leica
ACE600 high vacuum coater sputter. This coating minimizes the buildup
of electrostatic charge on the sample surface during imaging. Next, five
samples were placed in the electron chamber to observe the surface
directly. SEM images were obtained by JOEL IT-500HR with a beam
acceleration voltage of 5.0 kV and a working distance of 8.5 mm. For
each sample, three areas of observation were selected, where three
images with different magnifications (1000×, 5000×, and 10,000×)
were captured at each area. It should be noticed here that while SEM
images only capture the surface of the samples missing the underlying
microstructure features below the surface, the SEM images were used
comparatively (as discussed below) to validate the results of more
comprehensive microstructural experiments (e.g., SSA and MIP). Thus,
SEM images and data processing are considered valuable for the purpose
of this study.
Prior to image processing and estimating the pore size distribution
and circularity of the pores, the quality of the captured SEM images was
enhanced using ImageJ built-in filters (Rueden et al., 2017). First, mean
and median filters were applied to the picture to eliminate noises and
remove artifacts. These two spatial filters assess if a pixel is represen­
tative of its surrounding by comparing the pixel values in the vicinity
and replacing the value of the pixel of interest with the mean and then
the median of the considered neighborhood. Then, the contrasts of the
images were enhanced to signify the boundaries of pores and soil grains.
For the estimation of microstructural parameters, the images were
segregated into pores and solid domains. For this purpose, the thresh­
olding procedure was adopted in ImageJ software by selecting the lower
and upper thresholds to segregate the greyscale images into features of
5
Engineering Geology 318 (2023) 107101
interest. Finally, by assigning the appropriate scale values to the images,
pore areas and perimeters were estimated. Fig. 3 demonstrates the se­
quences of image processing. With the magnification presented in Fig. 3,
the pore size distribution for pores ranging from 10 nm to 2 μm can be
estimated.
By introducing the right scale to the images, the area of each pore
was calculated by ImageJ. Then, the SEM-based pore size distributions
were calculated from the measured pore areas by assuming the pores
have perfect circular shapes. With the magnification presented in Fig. 3,
the pore size distribution for pores ranging from 10 nm to 2 μm can be
estimated. Furthermore, the segregated images were used to calculate
the circularity of pores, which is defined by Eq. (7). The value of
circularity ranges from 0.0 for an elongated shape to 1.0 for a pore with
a perfect circular shape (Ferreira and Rasband, 2012).
Area
Circularity = 4π (7)
Perimeter2
3. Results and discussions
3.1. Macro-scale volumetric strain
Fig. 4 presents the calculated volumetric strains due to the me­
chanical and thermal loadings of each triaxial specimen. Table 1 sum­
marizes the calculated void ratios after consolidation (i.e., before
applying any thermal path) and at the end of the thermal path applied on
each specimen. All specimens experienced comparable volumetric
changes during the mechanical consolidation stage under the applied
400 kPa effective stress (Fig. 4.a). Furthermore, the various specimens
have comparable void ratios at the end of the mechanical consolidation
stage (i.e., before the thermal cycles) as shown in Table 1.
In fact, Fig. 4 aims to show that all of the considered samples expe­
rienced the same volumetric strains during the mechanical consolida­
tion stage (Fig. 4.a). These observations indicate that the mechanical
consolidation produced comparable specimens (e.g., fabric and pore
structure) prior to the initiation of the thermal stages. Therefore, the
consideration of the Isothermal Consolidation specimen as a reference,
representing the initial condition of all other specimens, is reasonable.
Also, similar volumetric strains were recorded for specimens subjected
to the same temperature changes (Fig. 4.b). This is critical to make sure
that we can actually consider each of the samples represents the path
experienced by the other samples, i.e., the changes in FTH sample were
also experienced by the FTHC samples over the first three thermal
stages.
As specimens' temperature decreases from 20 ◦ C to 0 ◦ C during the
initial phase of the freezing stage, negative pore pressures (i.e., cryo-
suction) develop within the specimens. The resulting suction triggers
water flow toward the triaxial specimen from the backpressure pump,
increasing the water content in the specimens. Subsequently, once the
temperature falls below freezing, ice forms in the pores expanding the
voids ratio and, consequently, the entire specimen (Morgenstern and
Nixon, 1971; Chamberlain, 1981; Eigenbrod et al., 1996).
Thawing, furthermore, generates excess pore pressures in the spec­
imens. The magnitude of this excess pore pressure depends on the soil's
ability to drain the thawed ice relative to the rate at which the excess
pore pressure is generated; the latter is directly correlated to the thawing
rate. The dissipation of the thawing-induced pore pressures under con­
stant confining stress is accompanied by a reduction in voids ratio, i.e.,
thaw-induced consolidation (Morgenstern and Nixon, 1971; Smith,
1972; Harris et al., 1995; Eigenbrod et al., 1996; Lesage, 2008; Yesuf
et al., 2013; Yao et al., 2017). Accordingly, the three triaxial specimens
that experienced thawing in this study (i.e., FT, FTC, and FTHC) showed
irreversible shrinkage (~1.15%) at the end of the freezing-thawing path
(Fig. 4.b).
Furthermore, as the soil temperature increases during the heating
stage for FTH and FTHC specimens, the higher thermal expansion
S.M. Zeinali and S.L. Abdelaziz
Fig. 3. The sequences of preprocessing of SEM images for the F sample as an example, a) raw image, b) mean filter, c) median filter, d) enhanced contrast, e)
segregated image.
coefficient of the pore water, relative to that of the soil particles and
skeleton, triggers water to seep out of the soil, causing additional
volumetric contractions of ~5.0% (Campanella and Mitchell, 1968;
Plum and Esrig, 1969; Baldi et al., 1988; Burghignoli et al., 1995;
Cekerevac and Laloui, 2004; Abuel-Naga et al., 2007b; Coccia and
McCartney, 2016; Tamizdoust and Ghasemi-Fare, 2019; Jaradat and
Abdelaziz, 2020; Zeinali and Abdelaziz, 2021). Finally, the FTHC spec­
imen underwent a slight expansion (~ − 0.9%) during the last cooling
stage. However, a permanent volumetric contraction (~7.2%) was
observed at the end of the full thermal cycle. This observation is in
accordance with previous studies on the response of normally consoli­
dated clays to heating-cooling cycles (Hueckel and Pellegrini, 1992;
Abuel-Naga et al., 2007a; Ng et al., 2014; Di Donna and Laloui, 2015;
Jaradat and Abdelaziz, 2020).
6
Engineering Geology 318 (2023) 107101
3.2. Specific Surface area (SSA)
Fig. 5.b presents the measured physisorption isotherms for the
sample obtained after the mechanical consolidation (i.e., the ISO sam­
ple). The existing hysteresis between adsorption and desorption
branches in Fig. 5.a is a result of bottleneck effects and cavitation of
liquid nitrogen during desorption (Thommes et al., 2015). Moreover, the
adsorption curve did not plateau as the relative pressure approached
1.0, which is attributed to the dominance of macropores (> 50 nm) as
supported by the MIP results in the previous section. Nevertheless, the
same overall shapes of the adsorption and desorption isotherms and
hysteresis loops were observed for other samples. The shape of the iso­
therms is closely correlated to the shape of the pores (Thommes et al.,
2015). According to IUPAC (Thommes et al., 2015) the adsorption and
desorption hysteresis shape is classified into six groups H1, H2(a), H2
(b), H3, H4, and H5, as shown in Fig. 5 (a). Accordingly, the shape of
obtained hysteresis in this study is comparable to H3. This type of
S.M. Zeinali and S.L. Abdelaziz Engineering Geology 318 (2023) 107101

(P-value) of the Shapiro-Wilk test for each sample. Since all the obtained
(a)
Time (min) P values are higher than the acceptable significance level, the null hy­
0.01 0.1 1 10 100 1000 pothesis is retained, and all datasets are considered normally
0 distributed.
In order to determine if the differences in the mean values were
’ statistically significant, we first performed F-tests to determine if the
3 = 400 kPa
2 datasets had equal or unequal variances. Each sample is tested against
the ISO sample, which is considered the reference sample in this study.
The obtained F values for each test are listed in Table 2. For all pairs of
samples 1 and 2 in a single F-test with equal sizes of N1 = N2 = 16, and a
Volumetric Strain (%)

4
ISO significance level of α = 0.05, Fcritical of 2.4 was calculated. Thus, the
F variances of all datasets were found to be statistically equal. Therefore,
6 FT two-tailed t-tests were performed, assuming equal variances, to deter­
FTH mine if the mean values were statistically different. For t-test the null
FTHC hypothesis was that the mean of two sets of measured specific surface
areas were not statistically different. The equal sample sizes and the
8
assumption of equal variance yielded to tcritical of 2.04. If the P-value
obtained based on the t-statistic is lower than the significance level α of
0.05, the null hypothesis was rejected. Therefore, considering the ISO
10
sample as the reference for the other samples which experienced the
different thermal paths, the specific surface area increased as the pores
expanded during freezing. However, the average specific surface area
12 after thawing for FT recovered to the initial value for ISO. For the FTH
(b) sample, the elevated temperature of 60 ◦ C decreased the specific surface
Volumetric Strain (%) area. Finally, at the end of the full thermal cycle, the specific surface area
-15 -10 -5 0 5 10 was reduced permanently for FTHC.
70
3.3. Pore size distribution
60

50 Figs. 6 and 7 present the total intruded and extruded mercury vol­
umes and the distributions of the throat and pore sizes for all considered
40 specimens. For a step-by-step comparison, the result of each sample is
plotted against all of its precedent samples. In this way, the effect of each
Temperature (°C)

30 temperature change is compared to the microstructural condition at the

Initial Temperature
20
20°C
10
0 Fig. 6.a to .c show the evolution of microstructure after freezing. The
-10
-20
-30
Fig. 4. Volumetric strains for the different specimens during (a) the mechanical
consolidation stage, and (b) the thermal path applied on each of the specimens.
hysteresis is associated with porous materials with plate-like aggregates
and slit-shaped pores with unrestricted absorption at high relative
pressures (Sing, 1982; Al Othman, 2012).
As discussed earlier, the BET method was utilized to estimate the
specific surface area (SSA) for each sample. Fig. 5.b shows the average
values along with the error bar represented by three times the standard
deviation indicating 99.73% of the data assuming a normal distribution.
The obtained results were compared using parametric hypothesis tests, t-
test, and F-test. The parametric hypothesis tests assume the distribution
of the population, which for the two tests in this study, the assumption is
that the data is drawn out of a population with normal distribution.
Therefore, before conducting these two tests and comparing the data set
statistically, the normality of each set was assessed by the Shapiro-Wilk
test (Shapiro and Wilk, 1965). The test was conducted to assess the null
hypothesis of normal population distribution and an acceptable signif­
icance level α of 0.05. Table 2 shows the Wstatistics, and significance level
end of the mechanical consolidation as well as the condition at the end of
the prior thermal stage. Also, the calculated modal throat and pore di­
ameters for each sample are summarized in Table 3.
3.3.1. Effect of Freezing
y-axes in Fig. 6.b and .c show the frequency of a given size in the sam­
ples. According to Fig. 6.a, the total volume of pores increased slightly
due to the expansion of the pore water upon freezing. The expansion
within the structure of the sample was previously observed by Othman
and Benson (1993), and Wang et al. (2020b, 2020c). The freezing-
induced expansion increased the modal throat size from 104.4 nm at
the end of consolidation to 110.08 nm. Furthermore, while the throat
size distribution for the Freezing sample shifts toward larger throats, the
curve for sizes more than ~370 nm lies beneath the one of ISO sample.
The diminished frequency of throats in this range can be interpreted as
either the collapse of the large throats under ice pressure, which resulted
in an increase in the frequency of smaller throats, or the migration of
pore water toward the freezing fringe. Additionally, the pores expanded
during freezing and thrust the pore size distribution toward pores larger
than the modal diameter, as shown in Fig. 6.c. However, the modal pore
size decreased from 750.20 nm to 691.02 nm. This observation suggests
that shrinkage and expansion of pores during freezing occur simulta­
neously, while some pores enlarged during expansion of pore water,
some other pores shrank due to water flow toward the freezing front. In
conclusion, freezing increased the total volume of voids increasing the
modal throat size, but decreasing the most frequent pore size.
3.3.2. Effect of freezing-thawing
Fig. 6.d to .f present the microstructural alterations from the
isothermal consolidation to the end of the freezing-thawing thermal
path. As shown in Fig. 6.d, the mercury intrusion curve for the FT sample

7
S.M. Zeinali and S.L. Abdelaziz Engineering Geology 318 (2023) 107101

Fig. 5. (a) IUPAC classification of isotherms (Thommes et al., 2015), (b) Adsorption and desorption isotherms for ISO sample, (c) evolution of specific surface area
with temperature.

Table 2
Shapiro-Wilk test, F-test, and t-test results of microstructural samples.
Samples Mean (m2/g) Variance Shapiro-Wilk test F-test t-test

Wstatistic P-value Fstatistic P-value tstatistic P-value

ISO 21.78 0.108 0.960 0.662

1.45 0.2402 3.52 0.0014
F 22.23 0.156 0.926 0.207
ISO 21.78 0.108
FT 21.67 0.221 0.892 0.060 2.18 0.0708 0.72 0.4764
ISO 21.78 0.108
1.25 0.3361 8.16 0.0000
FTH 20.88 0.086 0.968 0.809
ISO 21.78 0.108
2.28 0.0607 7.43 0.0000
FTHC 21.05 0.047 0.917 0.149

follows those for F sample for sizes larger than 300 nm. The two intru­
sion curves, however, deviate at smaller sizes (< 300 nm) with less total
intruded volume for the FT sample compared to the F and ISO samples.
This reduction in the intruded mercury volume for the FT sample sug­
gests an overall volumetric contraction, agreeing with that observed in
Fig. 4.b.
Additionally, the modal throat and pore diameters decreased at the
end of the thawing stage as shown in Fig. 6.e and .f, respectively. As
shown in Fig. 6.e, the throat size distribution for the ISO sample
generally agrees with that for the FT sample for sizes 350 nm or less;
however, the modal throat diameter in the FT sample is more frequent
compared to the ISO sample. For throats larger than 350 nm, it appears
that the FT sample preserved the same throat sizes as the F sample,
which were less than those in the ISO sample. Furthermore, there exists a
clear shift in the pore size distribution of FT sample toward smaller di­
ameters (Fig. 6.f). Yet again, the frequency of the modal pore diameter is
considerably higher than that for the ISO sample.
Zhang and Cui (2018) performed MIP on undisturbed samples

8
S.M. Zeinali and S.L. Abdelaziz Engineering Geology 318 (2023) 107101

Fig. 6. (a, d) Total intruded and extruded volumes of mercury and (b, e) throat and (c, f) pore size distributions from ISO to FT.

Fig. 7. (a, d) Total intruded and extruded volumes of mercury and (b, e) throat and (c, f) pore size distribution from ISO to FTHC.

9
S.M. Zeinali and S.L. Abdelaziz
Table 3
Modal throat and pore diameters.
Sample Modal throat size (nm) Modal pore size (nm)
ISO 104.40 750.20
F 110.08 691.02
FT 95.16 601.87
FTH 86.89 525.56
FTHC 93.21 708.50
collected from drilling holes in Shanghai. These samples were placed in
a container to undergo one cycle of freezing and thawing under no
external load. The MIP results by Zhang and Cui (2018) on the undis­
turbed samples before and after freeze and thaw reveal increases in both
the total volume of the pores and the modal throat size after thawing.
The same trend in the most frequent throat size was observed by Dalla
Santa et al. (2019) performing on soils consolidated one-dimensionally
in an oedometer and then subjected to freezing and thawing cycles.
The discrepancy among the results of this study with the findings of
Zhang and Cui (2018) and Dalla Santa et al. (2019) reflects the potential
dependency of the microstructural evolution of soils to the stress state.
3.3.3. Effect of freezing-thawing-heating
The continuation of heating after the thawing stage caused an
additional reduction in the total pore volume as shown in Fig. 7.a. Both
throat size and pore size distributions obtained from FTH moved toward
smaller sizes passing the distribution curves of the ISO sample. This
observation agrees with the typical macroscale contraction of normally
consolidated clays at elevated temperatures (Campanella and Mitchell,
1968; Plum and Esrig, 1969; Sultan et al., 2002; Abuel-Naga et al.,
2007a; Houhou et al., 2021; Loria and Coulibaly, 2021). Both the modal
throat and pore sizes were reduced upon heating. However, the fre­
quency of the modal throat size increased (Fig. 7.b) while the frequency
of the modal pore size remained the same (Fig. 7.c). This heating-
induced shrinkage of the pores was also reported earlier using 3-D to­
mography reconstruction from SEM images (Darbari et al., 2017).
3.3.4. Effect of freezing-thawing-heating-cooling
Moreover, subjecting normally consolidated and lightly over­
consolidated clays to a heating-cooling cycle results in irreversible
shrinkage despite the expansion during the cooling stage (Baldi et al.,
1988; Delage et al., 2000; Abuel-Naga et al., 2007b; Coccia and
Fig. 8. (a) The alteration of pore size distribution with thermal paths, and (b) distributions of SEM-based circularities.
10
Engineering Geology 318 (2023) 107101
McCartney, 2016). The same trend was observed in the microstructure
of the FTHC sample in this study as shown in Fig. 7.d. The total pore
volume (Fig. 7.d) and the modal throat (Fig. 7.e) and pore (Fig. 7.f)
diameters of the FTHC sample increased compared to those observed for
the FTH sample. However, the values at the end of consolidation (i.e., for
the ISO sample) were not retrieved and permanent microstructure
contraction was recorded for the FTHC sample.
3.4. SEM images
All calculated pore size distributions for the samples subjected to
thermal loadings are shown in Fig. 8.a. The curves before and after
freezing (i.e., ISO and F in Fig. 8.a) can be analyzed in two different
ranges of diameters, 1) pores larger than 500 nm, which experienced a
reduction in diameter due to freezing, and 2) pores smaller than 500 nm,
which increased in diameter after freezing. The same shrinkage of large
pores and expansion of smaller pores were observed in pore size distri­
bution measurements by MIP (Fig. 6 after freezing) and with a previous
study on the alteration of SEM-based pore size distribution due to
freezing by Darbari et al. (2017). While the expansion of pores was
anticipated due to the expansion of the pore water as ice forms, the
shrinkage of the large pores is associated with the collapse of these pores
under ice pressure or migration of pore water toward the freezing fringe,
as discussed in the analysis of the MIP results.
Furthermore, the pores generally shrank during thaw-consolidation
except pores smaller than ~50 nm, below which the initial pore size
distribution of Isothermal Consolidation sample was recovered. As the
temperature increased during the heating stage, the pores network
experienced further shrinkage. As per Fig. 8.a, an irreversible move to­
ward smaller diameters was estimated at the end of the full freezing-
thawing-heating-cooling cycle, which also is in a good agreement with
the overall shrinkage of normally consolidated clays after heating-
cooling cycles (Hueckel and Pellegrini, 1992; Bai et al., 2014; Jaradat
and Abdelaziz, 2020). However, the thresholding process involved in
the image processing along with the limitations of surficial observation
of the pores which prevents a full 3D capture of the pore network im­
poses some level of unreliability to the achieved pore size distributions.
Therefore, although the general evolution of the pore size distribution
with temperature assessed by SEM image processing agrees with that
observed by mercury intrusion porosimeter, the latter results are
considered more reliable.
S.M. Zeinali and S.L. Abdelaziz Engineering Geology 318 (2023) 107101

In addition, the circularity of the pores was calculated using Eq. (7). SEM-based circularity (C). This analogy supplements the conclusions
Higher calculated values of circularity means that the pores are closer to obtained from MIP, BET, and SEM imaging results and provides a sim­
perfect circles. Fig. 8.b presents the distribution of the estimated circu­ ple, yet comprehensive understanding of the microstructural alterations
larities for all samples considered in this study. The results are compared due to each of the thermal paths considered in this study. This analysis
using the effective circularities C10 and C60, the circularity values that demonstrates that the achieved microstructural parameters, namely
are exceeded by 90% and 40% of the pores, respectively. These values pore size distribution, specific surface area, and circularity are consis­
for each sample are summarized in Table 4. The results suggest that both tent if the number of pores is also changing accordingly. Therefore, the
freezing and thawing increased the effective circularity. However, number of pores is calculated using the original formulation of pore size
comparing C60, it appears that the total porous medium contained more distribution by MIP.
circular pores with higher circularity values after thawing. Furthermore,
compared to the effective circularity after thawing, C10 increased as the 4.1. Geometrical assessment of the pores
temperature increased to 60 ◦ C after freezing and thawing. However,
according to the alterations of C60 from FT to FTH, the portion of more A simple geometrical analysis is present by considering the ISO
circular pores with higher circularity decreased and recovered back to sample as stage n and the FT sample to stage k. The first boundary
the initial value of ISO. At the end of the full thermal cycle, the initial condition is given by Eq. (8).
porous medium transformed into a network consisting of more circular
pores, with higher effective circularity and C60. The elongation of pores rn > rk (8)
which is showcased in this study by higher circularity after thawing, From the mercury intrusion results, the second boundary condition is
agrees with Dalla Santa et al. (2019) X-μCT images obtained before and given by Eq. (9).
after freeze-thaw cycles. The increasing SEM-based circularity as well as
the continuous decrease in the modal pore size (Table 3) with the An > A k (9)
progress of the thermal cycle suggests that smaller pores possess higher Substituting the area of an ellipse into Eq. (9) yields Eq. (10).
circularity, although it requires more investigation.
nπ an rn > kπak rk (10)
4. Discussion: comparative microstructural assessment Thus, the ratio between the number of pores in the two stages is
given by Eq. (11).
Intuitively, there should exist a direct relation between the specific
n ak rk
surface are and pore size, meaning a larger pore should possess a higher > (11)
surface area. According to MIP results and SSA measurements, this k an rn
relation can be observed for F, FTH, and FTHC. At each of these samples, Furthermore, the statistical analysis of the measured specific surface
the specific surface area changed in the same direction of the change in area for the ISO and FT samples proved that thawing did not change the
modal throat size. However, in the sample after freezing and thawing specific surface area. Therefore, Pn = Pk. Utilizing the approximate
(FT), the measured SSA was similar to the initial value after consolida­ formulation of the circumference of an ellipse yields Eq. (12), which
tion measured in ISO sample. This inverse proportionality between SSA defines another relation for the ratio between the number of pores at the
and modal throat size suggests that other factors may control the specific two stages.
surface area, such as pore water flow. To better understand the observed √̅̅̅̅̅̅̅̅̅̅̅̅̅̅̅̅̅̅ √̅̅̅̅̅̅̅̅̅̅̅̅̅̅̅̅̅̅ √̅̅̅̅̅̅̅̅̅̅̅̅̅̅̅̅̅̅
behavior, the results of the specific surface area obtained by gas a2 n + r 2 n a2 k + r 2 k n a2 k + r 2 k
2nπ = 2kπ → = (12)
adsorption, pore size distribution measurements by mercury intrusion 2 2 k a2 n + r 2 n
porosimeter, and the deductions based on the circularity calculation by
SEM image processing are combined and incorporated into a simple Finally, the circularity increased from Isothermal Consolidation to
geometrical analysis. The evolution of the microstructure with thermal Freezing-Thawing as shown in Fig. 8.b. Thus, we can relate the di­
loadings was analyzed further, assuming the pores have simple ellipsoid mensions of the ellipses at the two stages using Eq. (13).
shapes. This particular shape was selected according to SEM images and πan rn πak rk
( √̅̅̅̅̅̅̅̅̅̅̅̅ )2 < ( √̅̅̅̅̅̅̅̅̅̅̅̅ )2 (13)
calculated circularities. In this analysis, the total number of pores at the 3 3 3 3
2π a n +r n
2π a k +r k
first stage was n, each of which has a minor axis of rn and major axis of 2 2

an, transforms into k number of pores with the minor and the major axes
of rk and ak, respectively, in the second stage. The area and circumfer­ Therefore,
ence of the considered ellipses are comparable to the pore volume and a k + r2 k ak rk
2

specific surface area, respectively. For this analysis, four boundary < (14)
a2 n + r2 n an rn
conditions were considered: 1) the relation between rn and rk defined by
the pore size distributions obtained from MIP, 2) the relative changes of Eqs. (11) through (14) suggest that, under the observed boundary
area (A) assessed by the total volume of intruded mercury, 3) the relative conditions, the number of pores is increased from the considered first
change of the perimeter of ellipses (P) from stage n to stage k achieved by stage (i.e., ISO) to that in the second stage (i.e., FT), as suggested by Eq.
specific surface area measurement using gas adsorption, and finally 4) (15).
the relation between definitive geometrical parameters assessed using √̅̅̅̅̅̅̅̅̅̅̅̅̅̅̅̅̅̅
a2 k + r2 k a2 k + r2 k n
< < 1→ < 1 (15)
a2 n + r 2 n a2 n + r 2 n k
Table 4
C10 and C60 obtained from SEM image processing and Number Ratio, the ratio of 4.2. Number of the Pores
number of pores of samples with respect to Isothermal Consolidation.
Samples C10 C60 NR The number of pores can also be estimated by extension of the
ISO 0.29 0.87 1.0 formulation of mercury intrusion pore size distribution. As discussed
F 0.36 0.87 5.1 earlier, the nominator of Eq. (4) (i.e., dV) is the total volume of pores for
FT 0.34 0.90 8.0 one interval of radius (ri-1 to ri+1). It is assumed that dV consists of ni
FTH 0.37 0.87 8.4 number of uniform pores with a radius of ri and volume of Vi. Therefore
FTHC 0.42 0.90 5.3
Eq. (4) can be expressed as shown in Eq. (16).

11
S.M. Zeinali and S.L. Abdelaziz
ni Vi
Dv (logr) = (16)
log(ri− 1 ) − log(ri+1 )
Eq. 16 yields the number of pores within one radius interval. The
summation of the estimated number of pores for each interval from MIP
results is the total number of pores per gram as given by Eq. (17).
j
∑ Dv (logr) × (log(ri− 1 ) − log(ri+1 ) )
nt = (17)
1
V
With the various assumptions and limitations attributed to mercury
intrusion porosimetry, such as the assumption of cylindrical pores and
the bottleneck effect discussed earlier, the values obtained from Eq. (17)
can only be used for a comparative study. For this purpose, the total
number of pores was calculated for each sample, and then its change
with respect to the ISO sample was expressed by the “Number Ratio”
parameter defined by Eq. (18).
nstage i
Number Ratio, NR = (18)
nISO
where i ranges from ISO to F, FT, FTH, and FTHC.
Table 4 lists the calculated values of the Number Ratio (NR) for each
of the considered samples. The observed trend suggests that freezing
increased the number of pores, which as discussed earlier, is an indi­
cation of the collapse of the macropores or pore water flow toward the
freezing front. Thawing increased NR, and further, the highest number
of pores is associated with the end of heating. During both of these two
stages, positive pore water pressure generates at the closed drainage
boundary of the triaxial specimens, from which all our microscale
samples were extracted. The thermally-induced pore water pressure
explains this increase in the number of pores. Nevertheless, although
from the end of the heating to the cooling stage, the number of pores
decreases, at the end of the full thermal cycle, an irreversible increase in
the number of pores was measured. In summary, during freezing, the
pores collapse under ice pressure and due to water flow inside the
sample. The positive pore pressure during thawing and heating increases
the number of pores further. Finally, the negative pore pressure during
cooling merges some pores with one another, but the resulting medium
still has more pores relative to its initial condition.
5. Conclusion
In this study, the effect of a full thermal cycle on the microstructure
of clay was evaluated. For this purpose, one saturated clay specimen was
only subjected to mechanical consolidation under an effective stress of
400 kPa, as a reference specimen representing the initial microstructural
condition for other specimens. Four more kaolinite clay specimens were
saturated and consolidated under similar effective stress and then sub­
jected to four different temperature changes complementing a full
thermal cycle. Therefore, each sample represents the microstructural
condition at the end of each stage within the thermal cycle. The
considered thermal cycle contains four stages, namely freezing (20 ◦ C to
− 15 ◦ C), thawing (− 15 ◦ C to 20 ◦ C), heating (20 ◦ C to 60 ◦ C), and
cooling (60 ◦ C to 20 ◦ C). All the mechanical and thermal loadings were
applied under a single drainage condition with free drainage at the top
of the sample. Once each specimen completed its corresponding stages
of mechanical and thermal loadings, two thin disks of soil were cut from
the bottom height of specimens and then were flash-frozen in liquid
Nitrogen and freeze-dried to preserve the microstructure. Samples were
then obtained from dried soil disks for microstructural analysis. First,
the change of pore size distribution was assessed by mercury intrusion
and extrusion porosimetry. Then, the alteration of specific surface area
at each stage of a thermal cycle was evaluated by gas adsorption technic.
Multiple measurements of specific surface area were conducted on the
samples obtained from various locations of each disk. Then, the datasets
were tested for normality. Next, the mean values of data sets were
12
Engineering Geology 318 (2023) 107101
compared using t-test. Furthermore, the porous structure for each
specimen was captured by scanning electron microscope, and the images
were analyzed by image processing methods for estimation of SEM
based pore size distribution and circularity. Next, all the obtained
microstructural parameters were incorporated into a comparative study
of the pore shapes to quantify the microstructural changes of samples
with temperature.
The results showed that:
• The pores become more circular under the thermal load as observed
by SEM images; this behavior was observed for all of the considered
thermal paths.
• As a consequence of the expansion of pore water and collapse of
larger pores, as well as the seepage of water out of large pores toward
the freezing front, the modal throat and pore sizes, increased and
decreased, respectively. However, the specific surface area
increased. All are resulting in an increase in the number of pores at
the end of freezing.
• During thawing consolidation, both throats and pores shrank to a
smaller value of the initial microstructural condition, after me­
chanical consolidation. However, at the end of the thawing stage, the
initial value of the specific surface area was recovered.
• With increasing the temperature after thawing to 60 ◦ C, the modal
throat and pore size decreased further. Also, the specific surface area
at the end of the heating stage was less than the initial value. How­
ever, the consolidation and collapse of pores under the thermally
induced pore water pressure due to heating increased the number of
pores.
• With cooling the sample temperature to the initial value of 20 ◦ C, a
permanent shrinkage of the modal throat and pore sizes and a re­
sidual reduction of specific surface area was observed. Nevertheless,
the number of pores remained 5.3 times higher than that of after
mechanical consolidation.
The findings of this study will allow more robust estimates of the
evolution of the thermal and physical properties of cohesive soils sur­
rounding geothermal heat exchangers and thermo-active geostructures.
Changes in the pore structure will result in changes in the relative
proportions of the constituents of the soils, which consequently will alter
the thermal and physical properties of the soil, sometimes significantly.
Furthermore, changes in the pore structure may cause significant
changes in the hydraulic conductivity of the soil as pores become more
or less connected together, changing the thermally-induced water flow
around geothermal heat exchangers. Thus, these results pave the road
for more reliable designs of shallow geothermal systems. Furthermore,
the obtained results and conclusions can be exploited to seek the origins
of thermal macroscale behavior, which enables the geotechnical engi­
neers to modify the earthen materials and thermal soil stabilization
methods to mitigate unfavorable consequences of temperature change in
soil behavior. The results can also be further utilized to validate porous
network and DEM models, increasing the efficacy of these predictive
tools to deduce the thermal response of grounds in geotechnical appli­
cations. It should be noted that the observed microstructural evolutions,
namely pore size distribution, specific surface area and circularity, as
well as the concluded points, are only applicable for the normally-
consolidated clay samples with Kaolinite minerals subjected to one
isotropic consolidation stress and all-around temperature changes. The
effect of different consolidation stresses, different stress histories, and
different thermal paths requires more investigation.
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.
S.M. Zeinali and S.L. Abdelaziz
Data availability
Data will be made available on request.
Acknowledgment
This material is based upon work supported by the U. S. Army
Research Laboratory and the U. S. Army Research Office under contract
numbers W911NF-16-1-0336, W911NF-17-1-0262, W911NF-18-1-
0068, and W911NF-20-1-0238. The discussions and conclusions pre­
sented in this work reflect the opinions of the authors only.
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