Influence of Temperature and Duration of Thermal

Treatment on Properties of Excavated Soil

as Fine Aggregate in Cement Mortar
P. Priyadharshini, Ph.D. 1; K. Ramamurthy, Ph.D., M.ASCE 2; and R. G. Robinson, Ph.D. 3
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Abstract: In the interest of utilizing high-plasticity excavation soil as a replacement for fine aggregate in cement mortar, a study on the
thermal treatment of soils containing 25% and 40% clay fractions was carried out. A range of tests including thermogravimetric analysis
(TGA) and X-ray diffraction (XRD) were conducted to examine the transformation of fines (silt þ clay) in soil at temperatures ranging from
200°C to 1,000°C. Thermally treated soils were used as fine aggregate in cement mortar, and properties such as water demand, dry density,
compressive strength, and drying shrinkage were studied. The experiments were designed with the parameters treatment temperature
and duration using central composite design of response surface methodology. From the test results, it was concluded that thermal treatment
helps in transforming clayey soil, even high-plasticity soil, to be used as a suitable fine aggregate material in cement mortar. However, the
properties of thermally treated soil highly depend on the clay mineralogy present in it. DOI: 10.1061/(ASCE)MT.1943-5533.0002759.
© 2019 American Society of Civil Engineers.
Author keywords: Clay; Plastic soil; Thermal treatment; Shrinkage; Cement mortar; Fine aggregate.

Introduction
Due to continuous depletion of river sand, crushed stone has been
growing in popularity as a suitable fine aggregate replacement.
Treatments such as sieving, washing, and granulometric propor-
tioning have become common for high-quality crushed aggregate
(Khouadjia et al. 2015; Cepuritis and Mørtsell 2016). Other sources
of fine aggregate alternatives are industrial by-products and wastes
such as recycled fine aggregate, foundry sand, quarry dust, slag,
and bottom ash. These materials, when directly used in concrete,
affect the fresh and hardened properties. There are few works sug-
gesting one or more treatments for such alternative fine aggregates
to produce concrete with properties comparable to those of concrete
with river sand (Cepuritis and Mørtsell 2016; Purushothaman et al.
2015; Priyadharshini et al. 2018b). Some of the treatment methods
adopted were washing and/or sieving to remove excessive fines.
However, a granulometric adjustment was needed for washed
marine sediments to achieve properties equivalent to those of river
sand (Couvidat et al. 2016; Ozer-Erdogan et al. 2016). Similar
observations were made by Priyadharshini et al. (2018b) regarding
washed excavation soils of varying particle size distributions; the
1 down to desirable limits (Priyadharshini et al. 2018a).
Formerly, Doctoral Research Scholar, Building Technology and
Construction Management Division, Dept. of Civil Engineering, Indian
Institute of Technology Madras, Chennai 600036, India. ORCID: https://
orcid.org/0000-0002-7731-2016. Email: mail2pridha@gmail.com
2
Professor, Building Technology and Construction Management
Division, Dept. of Civil Engineering, Indian Institute of Technology
Madras, Chennai 600036, India (corresponding author). ORCID: https://
orcid.org/0000-0001-6177-6230. Email: vivek@iitm.ac.in
3
Professor, Geotechnical Engineering Division, Dept. of Civil Engi-
neering, Indian Institute of Technology Madras, Chennai 600036, India.
Email: robinson@iitm.ac.in
Note. This manuscript was submitted on August 18, 2018; approved on
January 15, 2019; published online on May 20, 2019. Discussion period
open until October 20, 2019; separate discussions must be submitted for
individual papers. This paper is part of the Journal of Materials in Civil
Engineering, © ASCE, ISSN 0899-1561.
soil with gradations similar to that of river sand produced compa-
rable results. Chemical treatment with hydraulic binders such as
lime were also used to stabilize materials with clay content such
as marine sediments. Though thermal treatment involves energy
consumption, marine sediments thermally treated at a temperature
of 450°C exhibit significant improvement in material properties
(Sannier et al. 2009).
A huge volume of excavation soil is generated from construction
sites, tunneling works, surface mining, and other deep excavations.
However, the potential use of excavation soil as a fine aggregate
alternative is unexplored, probably due to the soil’s silt and clay
content. Washing seems to be effective for removing the fine frac-
tion, but it cannot be employed for excavation soil with high-
plasticity (HP) clay, which clogs the sieves and needs frequent
cleaning. In such cases, stabilization of the clay is an alternative
that has been adopted largely in geotechnical engineering applica-
tions (Brooks et al. 2011). Eid (2017) applied this technique in raw
earth with 25% silt (0% clay) as a construction material, and found
that it helped in reducing shrinkage strains. However, stabilization
has its own limitations on the amount and mineralogical composi-
tion of clay in the soil. When the percentage of HP clay exceeds
25%, shrinkage of mortar with stabilized soil cannot be brought
Hence, there is a need for an appropriate treatment for materials
containing high amounts of HP clay. Thermal treatment is an age-
old ground improvement technique to avoid differential settlement
of weak clayey soils; unlike other methods, it produces immediate
results (Litvinov 1960; Wang et al. 2008). In this study, tempera-
tures in the range of 100°C to 200°C were employed to drive
away moisture in the soil as a way to improve soil strength. The
pozzolanicity of clay minerals such as kaolinite, illite, and mont-
morillonite was enhanced with heat treatment in the range of 600°C
to 800°C, improving the chemical interaction of soil aggregate and
binder (Zhang and Gjørv 1990). This material was explored for
its potential as a cement replacement material (Fernandez et al.
2011). Sintering of clayey soil and particle growth result from treat-
ment temperatures beyond 900°C, providing granular material that

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 retains its compressive strength under wetting and drying condi-
tions. It has been suggested as an economic substitute for gravel
and crushed rock to avoid importing construction materials at high
costs (Joshi et al. 1994).
In this study, locally available soils of medium and high plas-
ticity were chosen and treated thermally. Cement mortar properties
with thermally treated soils were compared with mortar with un-
treated soil and control mortar with river sand. Thermogravimetric
analysis (TGA), X-ray diffraction (XRD), and particle size distri-
bution of the treated soils were used to understand their struc-
tural changes and were correlated to the effect of thermally treated
soil on cement mortar properties such as compressive strength
and drying shrinkage. Changes in porosity and pore refinement
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due to thermal treatment were studied with mercury intrusion
porosimetry (MIP).
Materials and Methods
Two types of locally available excavation soil, medium plasticity
(MP) and HP, with 48% and 58% fines (silt and clay), respectively,
were used in this study. Combinations of kaolinite, illite, and mont-
morillonite clay minerals in these soils, gave them varying plasticity
characteristics. MP and HP soils fall into the category of clayey sand
and fat clay according to ASTM D2487 (ASTM 2017a), with a spe-
cific gravity of 2.61 and 2.56, respectively. The surface area of the par-
ticles passing a 75-μm sieve varied between 265 and 303 m2 =g. There
was wide variation in the free swell index of the soils, with 15% for MP
and 300% for HP due to the type of clay mineral each contained.
Thermogravimetric Analysis
Soil samples passing a 75-μm sieve were used to characterize
the thermal behavior of fines content in the soils using a SDT
Q600 thermogravimetric analyzer (TA Instruments, New Castle,
Delaware). The samples were heated at a rate of 20°C=min, and
the temperature was ramped from ambient to 1,200°C in a nitrogen
environment. Changes in mass and heat flow with the rise in
temperature were recorded.
Thermal Treatment
The soil samples were thermally treated in a muffle furnace at tem-
peratures of 200°C, 400°C, 600°C, 800°C, and 1,000°C, increasing
at a rate of 5°C=min from room temperature. Once the desired tem-
perature was reached, it was held for 30 to 180 min. The samples
were then allowed to cool and used for further characterization and
mortar preparation.
Characterization of Thermally Treated Soil
Thermally treated samples were characterized for their mineralogi-
cal changes using a PANanalytical X’Pert Pro XRD spectrometer
with Cu-Kα as the source (Malvern Panalytical, Malvern, UK).
A slit width of 6 mm with a step scan size of 0.02°/sand a counting
time of 20 s was adopted. The completely dried raw soil and ther-
mally treated soils were sieved through a 50-μm sieve, and the pow-
der samples were used for testing. The XRD patterns were identified
with the International Crystal Structure Database (ICSD 2009).
Quantitative determination of particle size distribution of the
finer portions of the soils was achieved using hydrometer analysis
per ASTM D7928 (ASTM 2017c). The analysis was repeated three
times for each sample, and average values were taken. Bulk density
and percentage of voids were calculated for these samples per
ASTM C29 (ASTM 2017b).
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Mortar Preparation
The ratio of fine aggregate to cement was fixed at 3 (by weight) for
mortar preparation. Ordinary 53-grade portland cement, conform-
ing to IS 12269 (BIS 2013), was used as a binder. Well-graded river
sand was used as the fine aggregate in the control mortar speci-
mens. Initially, the cement mortar was cast with untreated soils and
river sand to serve as a benchmark in evaluating the relative per-
formance of the treated soils’ mortar properties. The workability of
the mortar was measured using flow percentage in three trials for
each mix per ASTM C1437 (ASTM 2015). The amount of water
required to maintain a constant flow of 110%  5% was determined
and noted as the water demand. For each mortar mix, 15 50-mm
cube specimens (3 for dry density, 6 for compressive strength, and
3 for porosity) were cast. In addition, 3 prism specimens of size
160 × 40 × 40 mm were cast for shrinkage measurements.
Mercury Intrusion Porosimetry
Permeable pore volume and critical pore size distribution in the
mortar specimens were calculated via MIP. After 28 days of curing,
the specimens were sliced into 5-mm pieces using a diamond saw
cutter and stored in isopropanol for 7 days to stop hydration by the
solvent exchange method. The sliced specimens were then dried in
a vacuum desiccator for a minimum of 4 days until testing. For each
mix, 3 to 4 5-mm pieces were chosen to give better accessibility
to MIP. A Pascal 440 instrument with a maximum pressure of
440 MPa, which can sense pores as small as 3 nm, was used
(ThermoFisher Scientific, Waltham, Massachusetts). The Washburn
equation is given as
4γ cos θ
D¼−
P
which relates the pore diameter (D) at different pressure levels (P)
with the surface tension of the mercury (γ); the cosine of the contact
angle (θ) was used to interpret the MIP data.
Properties of Thermally Treated Soil
Mineralogical Properties
The effect of heat treatment on the mineralogical composition of
MP and HP soils can be explained through the XRD pattern shown
in Figs. 1(a and b). I MP soil is mainly composed of montmoril-
lonite, illite, and stilbite [Fig. 1(a)], whereas HP soil is predomi-
nantly composed of montmorillonite and illite [Fig. 1(b)].
Both MP and HP soils showed montmorillonite/illite peaks at
600°C, indicating that dehydroxylation was not complete at this
temperature. The structural decomposition of the clay minerals was
clearly visible from the disappearance of its peak at 1,000°C. MP
soil, in addition to montmorillonite/illite showed peaks of stilbite,
which remained stable during thermal treatment without mineral-
ogical changes and remained crystalline even at 1,000°C.
Physical Properties
Figs. 2 and 3 respectively show the transition in size of the clay and
silt particles established through hydrometer testing of the MP and
HP soils, as well as the corresponding changes in the soils’ other
physical properties. Heating the soil samples to 200°C increased the
clay-sized particles irrespective of soil type because of the reduc-
tion in grain size due to shrinkage caused by dehydration, sup-
ported by the mass loss of MP and HP soils obtained through TGA
(Fig. 4). Change in the mass of a sample was due to dehydration,
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Fig. 1. XRD pattern of untreated and thermally treated soils: (a) MP soil; and (b) HP soil.

Fig. 2. Physical changes in thermally treated MP soil: (a) transition from clay to silt; and (b) bulk density and voids percentage.

Fig. 3. Physical changes in thermally treated HP soil: (a) transition from clay to silt; and (b) bulk density and voids percentage.

decomposition, or oxidation. The mass loss in the temperature clay present. Here, HP soil with montmorillonite showed the higher
range of 50°C to 200°C indicated dehydration due to loss of free mass loss at this temperature range compared with MP soil (Fig. 4);
water between the clay layers. Dehydration loss generally is rela- the initial increase in the clay-sized fraction at 200°C was higher
tively higher in HP soil than in MP soil owing to the amount of (4%) in comparison also [Fig. 3(a)]. Similar results were observed

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Fig. 4. TGA curves for soil samples.
by Wang et al. (1990) when dry kaolinite and montmorillonite clay
samples were subjected to heat treatment at temperatures ranging
from 100°C to 400°C.
Increasing the treatment temperature beyond 200°C reduced
both silt- and clay-sized particles due to dehydroxylation; this was
followed by the growth of these particles. Dehydroxylation loss
was due to the removal of structural water from the clay mineral.
For kaolinite, dehydroxylation occurred at 400°C–600°C, as clearly
observed in both the MP and HP soils, with a loss in mass at
this temperature range (Fig. 4). In this case, dehydroxylation breaks
the inter-layer hydroxyls binding, which caused the deformation of
crystalline structure (Fernandez et al. 2011). The dehydroxylation of
montmorillonite occurred at temperatures ranging from 600°C to
800°C, with a corresponding mass loss in this temperature range for
HP soil (Fig. 4), as indicated by the reduction in fines from 48% to
30% in MP soil and 58% to 32% in HP soil [Figs. 2(a) and 3(a)].
In HP soil, the presence of montmorillonite clay with adsorbed
water resulted in greater reduction in fines totaling. 18% to 26%;
however, in spite of the reduced number of clay-sized particles,
there was also a 10% increase in silt-sized particles. Yilmaz (2003)
and Wang et al. (2008) attributed this phenomenon to the removal
of adsorbed water around the clay particles which brought them
together, thus favoring an increase in in clay particle size up
to the size of the silt-sized particles. Generally, bulk density is
higher for HP soil, indicating the efficiency of thermal treatment
[Figs. 2(b) and 3(b)]. The increase in silt-sized particles with a
corresponding reduction in clay-sized particles between 800°C
and 1,000°C is due to the sintering effect at high temperatures
[Fig. 2(a)].
Behavior of Cement Mortar Containing Thermally
Treated Soil
Treatment temperature and duration were the two parameters con-
sidered in this study. Each parameter had five levels within the fixed
range: 200°C to 1,000°C and 30 to 180 min, respectively. The TGA
curve in Fig. 4 shows changes in the clay structure from 200°C
to 800°C, making 1,000°C the maximum treatment temperature.
Treatment duration was based on trials; to make the treatment
energy efficient, the minimum duration was set at 30 min. Ex-
periments followed the central composite design (Montgomery
2012) of response surface methodology (RSM), with 13 sets of
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Table 1. Factors in uncoded values for coded values of the parameters
studied
Coded values
þ1.414 þ1 0 −1 −1.414
Parameter Uncoded values
Temperature (°C) 200 317 600 882 1,000
Duration (min) 30 51 105 158 180
experiments (for each MP and HP soil). The coded and uncoded
values of the parameters are given in Table 1.
In RSM problems, the response and the independent variables
are related using a quadratic model of the form
X
k X
k XX
y ¼ b0 þ bi xi þ bii x2i þ bij xi xj
i¼1 i¼1 i<j
where, xi (i ¼ 1; 2 : : : k) = quantitative variables; and bi , bj = least-
squares estimates of the regression coefficients.
The model equations for MP and HP soils are given in
Appendix I. Analysis of the experimental data was carried out
using SAS 8.02; the regression models contained terms that were
statistically significant (those that had a T-statistics greater than
that of the chosen significance level of 0.05) and were used to ob-
tain the response surface. The statistical model was validated based
on R2 , P-values, and F-values in the output data as given in
Appendix I. R2 was found to be > 0.9 for most of the responses,
which gave confidence in applying the predicted model and could
be used for analyzing the responses for different combination of
parameters within the mentioned range. Models were found stati-
cally significant if their P-value lay within 0.05. The ANOVA
results for water demand, dry density, compressive strength, dry-
ing shrinkage, and permeable pore volume are summarized in
Appendix II for MP and HP soil, respectively. The factors influenc-
ing the mortar properties were significant if their P-value were less
than 0.05.
Water Demand for Constant Workability
Fig. 5 presents the variation in water demand for achieving con-
stant workability of mortar with thermally treated soil. For a con-
stant temperature, the duration of thermal treatment did not affect
the water demand significantly—that is, approximately 50 kg=m3
[Fig. 5(b)]. However, an increase in treatment temperature resulted
in a significant reduction in water demand, due to the increase in
clay particle size with increasing treatment temperature which re-
quired less water content for workability. This effect was higher
in HP soil with high clay content [Fig. 5(a)] and could be attributed
to the reduction in interlayer space between the clay particles,
which aided sintering and particle growth [Figs. 3(a and b)].
It agreed with the finding of Warshaw et al. (1960) that the X-ray
diffraction pattern of natural layered silicates with different clay
minerals, thermally treated at a temperature range of 400°C to
500°C for 12 h shows destroyed layers and reduced layer space.
HP soil with 41% clay content treated at 1,000°C could reach a
water demand equivalent to that of river sand due to the reduction
in clay content from 41% to 4% at this temperature [Fig. 3(b)].
It shows that thermal treatment is effective for soil with montmo-
rillonite and improves the properties of HP soil for use as fine
aggregate.
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Fig. 5. Water demand in cement mortar with thermally treated soils: (a) MP soil; and (b) HP soil.

Dry Density
The dry density of cement mortar with thermally treated MP
and HP soil as fine aggregate is shown in Fig. 6. At a given
duration, when the treatment temperature varied from 200°C to
1,000°C, there was a 35% and a 68% increase in dry density for
mortar with MP and HP soil, respectively. The growth of clay-sized
particles increased with plasticity, resulting in a reduction in water
demand as indicated by the density increase. This could also be
related to the reduction in void ratio and the increase in bulk density
with treatment temperature for the thermally treated soil samples
[Figs. 2(b) and 3(b)]. Both soils, when treated at about 800°C for
180 min and used as fine aggregate in cement mortar, attained a dry
density of 1950  50 kg=m3 .
At a constant temperature, the dry density of mortar with ther-
mally treated soil increased by an average of 10% with increasing
treatment duration from 30 to 180 min. The effect of duration in-
creased with increasing temperature and reached its maximum at
1,000°C, because the montmorillonite in the plastic soils required
sustained heating at high temperatures (>600°C) for complete
decomposition, though the reduction in clay lamellar space at lower
temperatures also had some effect (Sarikaya et al. 2000).
Compressive Strength
The compressive strength of the cement mortar with thermally
treated MP and HP soil is compared with that of mortar with river
sand and untreated soils in Fig. 7. For a constant treatment duration,
the compressive strength of thermally treated MP soil increased
with increasing temperature [Fig. 7(a)]. However, it attained only
67% of the compressive strength of mortar with river sand at
1,000°C for 180 min, perhaps because of the proportion of illitic
clay in the MP soil, which did not respond to the thermal treatment
below 1,000°C as shown in the XRD curves in Fig. 1(a). This
response of illitic clay to thermal treatment was also reported by
Bhatnagar and Goel (2002) in alluvial deposits of Indo-Gangetic
plains of India.
The compressive strength of mortar with thermally treated HP
soil increased with treatment duration and temperature [Fig. 7(b)].
This increase was linear from 200°C to 1,000°C. The large volume

Fig. 6. Dry density of cement mortar with thermally treated soils: (a) MP soil; and (b) HP soil.

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Fig. 7. Compressive strength of cement mortar with thermally treated soils: (a) MP soil; and (b) HP soil.
of montmorillonite in the HP soil required high a treatment temper-
ature for complete disintegration of its structure. Additionally, at
high temperatures pore refinement was shown to be better in reac-
tive clay [Fig. 3(b)] and to improve strength compared to nonex-
pansive clay. This effect is supported by a comparative study on
heat treatment of kaolinite and montmorillonite at 100°C to 900°C
(Joshi et al. 1994), and may have been the reason for the signifi-
cantly improved strength in mortar with HP soil, which exceeded
the strength of mortar with river sand at 1,000°C. This strength im-
provement of MP and HP soil was also due to the reduction in water
demand with thermal treatment (Fig. 5). The higher the response of
the soil to treatment, the greater the improvement in mortar proper-
ties. Mortar with HP soil reached a water demand as low as that
of river sand at 1,000°C, which explained its strength performance
exceeding that of other mixes.
The ratio of strength to density of cement mortar with thermally
treated MP and HP soil is compared with that of mortar with river
sand in Fig. 8. Though the ratio for mortar with MP soil increased
from 0.4 to 1.4, it did not reach a value as significant as that of
Fig. 8. Strength–density ratio of cement mortar with thermally treated
soils.
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mortar with HP soil. This could be attributed to the temperature
requirement to activate illite, which is why there was a marked
difference in the effect of duration only at a 1,000°C, and to the
improvement in bulk density and reduction in void ratio, which was
higher for HP soil (Fig. 4). The ratio of strength to density for HP
soil was widespread and exceeded that for mortar with river sand at
1,000°C. The spread in the ratio for HP soil shows its significant
improvement in strength with increasing treatment temperature,
which is attributed to the presence of montmorillonite, as shown by
XRD and TGA curves [Figs. 1(b) and 2(b)]. Mortar with thermally
treated HP soil showed strength comparable to the strength of
mortar with river sand at a lower corresponding density range
(1,800 to 2,000 kg=m3 ).
Drying Shrinkage
The drying shrinkage strain of mortar with thermally treated MP
and HP soil is compared with those of the mortar containing un-
treated soils and the control mortar with river sand in Fig. 9. The
drying shrinkage strain of mortar with MP and HP soil reduced by
85% and 95%, respectively, when the treatment temperature rose
from 200°C to 800°C. This was because of the reduction in clay-
sized particles with increasing temperature in both soils (Fig. 3).
Egan et al. (2017) mentioned increased aggregate volume as a
possible parameter in altering shrinkage strain. Here, increasing
temperature aided the sintering of the clay particles and the growth
in particle size, thus helping to reduce shrinkage of mortars with HP
soil. However, there was an average increase of 10% in drying
shrinkage strain at 1,000°C for mortars with MP and HP soil
[Fig. 9(b)], due to the critical pore size distribution in the hardened
mortar.
Critical pore size distribution was calculated from MIP data.
From the MIP curves of the hardened mortar with MP and HP soil,
mortar with untreated soils showed three to four critical pore diam-
eters without definite shape, which looked more like a MIP curve of
a plain soil specimen. MIP curves of mortar with thermally treated
MP and HP soils showed bimodal curves typical of a cement mortar
specimen [Fig. 10(a)]. There was a reduction in pore size with
thermal treatment that helped in bringing down the shrinkage
strains. However, it must be stressed that an increase in the reac-
tivity of clay particles with the application of thermally treated MP
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Fig. 9. Drying shrinkage of cement mortar with thermally treated soils: (a) MP soil; and (b) HP soil.

Fig. 10. Pore size distribution curves for cement mortar: (a) river sand; (b) MP soil; and (c) HP soil.

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Fig. 11. Permeable pore volume of mortar with river sand.
[Fig. 10(b)] and HP soil [Fig. 10(c)] at 1,000°C resulted in more
hydration products and hence the formation of nanopores. This
caused an increase in shrinkage strain at this treatment temperature.
Permeable Pore Volume
The permeable pore volume and the differential intrusion volume
from the MIP curve in Fig. 11 gives the total permeable porosity.
Permeable porosity of mortar/concrete is considered to be the main
factor governing the durability of the material through which water/
aggressive chemicals enter hydration products.
The influence of treatment temperature and duration on per-
meable pore volume in the hardened cement mortar with thermally
treated MP and HP soil is shown in Fig. 12. The reduction in per-
meable porosity gives a clear picture of improvement in the proper-
ties of mortar containing thermally treated soil. For any soil type,
total mortar porosity decreases with increasing treatment temper-
ature. This can be related to the growth in particle size with increas-
ing temperature which alters the particle size distribution; thereby,
the porosity (voids content) of mortar decreases.
At a treatment temperature of 1,000°C and a duration of
120 min, mortar with MP soil produced a microstructure with the
Fig. 12. Permeable pore volume of cement mortar with thermally treated soils: (a) MP soil; and (b) HP soil.
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least permeable pore volume [Fig. 12(a)]. For mortar with HP soil,
porosity was affected by both temperature and treatment duration.
There was a marked reduction in permeable pore volume with in-
creasing duration at any given temperature. HP soil with almost
50% clay content responded well to heat treatment and, the modi-
fication of its crystal structure occurred gradually with increasing
duration [Fig. 12(b)]. Mortar with HP soil achieved porosity even
below that of the control mortar when treated at >800°C for
120–180 min.
Embodied Energy
As thermal treatment method involves high temperature, it was im-
perative to compare the embodied energy of the processed material
with that of the conventional fine aggregates currently used in con-
struction industries. In order to illustrate the methodology, here
a jobsite is assumed to be located in Chennai, Tamilnadu (India).
The nearest available river sand for a construction site in Chennai
is in Chengalpattu (62 km). For extraction of loose material like
river sand, a mechanical shovel operating on diesel (energy−
43.1 MJ/kg) is used (da Rocha et al. 2016). A potential replacement
for river sand that is already accepted in construction industry is
crushed stones. Production of crushed stone involves various proc-
esses such as mining, crushing, sieving, washing, and proportioning.
The energy involved in these operations is calculated from available
data in the literature and equipment manuals (Landfield and Karra
2000). Rock mining involves percussion drills, hydraulic shovels,
dump trucks, and bulldozers (EEP 2013). The crushed stone aggregate
quarry nearest to Chennai city is Sriperumbudur (40 km). It is known
that natural sand/crushed stone consumes 1.75 MJ=m3 of energy for
every 1 km of transport distance (Reddy and Jagadish 2003).
Embodied energy analysis of a construction material employs
one of several approaches for comparing different compositions.
In this study, drying shrinkage strain was considered to be the most
important parameter because fine aggregate plays an influential role
in the shrinkage of soil-based mortar. Cement mortar, which under-
goes a shrinkage strain equivalent to that of mortar with river sand,
was used as the reference to fix the studied parameters of alterna-
tive fine aggregates (excavation soil). Based on the experimental
data, these parameters were fixed at 800°C for 120 min for MP and
HP soil. Additionally, 90 min. of treatment was considered for
both soil types, giving a shrinkage strain less than 2,000 μstrains.
J. Mater. Civ. Eng.
 Table 2. Comparison of embodied energy of conventional and alternative fine aggregates
Processing Transportation
Fuel Fuel Production Energy Distance Energy Total embodied
Fine aggregate Category type consumption (Mg=h) (MJ=Mg) (km) (MJ=Mg) energy (MJ=Mg)
River sand Extraction Diesel 0.15 L=h 143 54.00 62 108.5 162.5
Crushed stone Extraction Diesel 15 L=h (For granite) 182.67 40 70 255.47
Crushing Electric — 100 1.60 — — —
Screening Electric 27 MJ=h 50 0.20 — — —
Washing Electric 54 MJ=h — 1.00 — — —
Excavated soil ð0.45–0.6Þ kJ=kg · °C × ð800°C Electric 27 MJ=h 0.41–0.65 81–162 40–60 70–122.5 151–284.5
for 90–180 minÞ
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An industrial-grade electrical furnace with a capacity of 500 kg=h
and power consumption of 27 MJ=h was used for the energy and
cost calculations of the thermal treatment of the different soils. It
was found that the thermal conductivity derived from soil sample
calorimetric data increased with fineness and clay content. This is
found to be in the range of 0.45–0.6 kJ=kg°C for MP and HP soil.
The transportation of excavated soil is from the construction site
to the treatment plant and from the plant to the site. Considering a
treatment plant on the fringes of a city, the maximum transportation
distance for excavated soil before and after treatment could be
40 km. The embodied energy comparison in this study was based
on gate-to-gate and is presented in Table 2. Also, processing of
crushed stone requires nonrenewable fuel such as diesel/electricity,
which cannot be replaced by alternative energy.
Though there may be a marginal increase in embodied energy of
the thermally treated soil based on its characteristics, it is important
to study potential alternatives for fine aggregate based on current
industry need.
Conclusions
The following conclusions are applicable to the range of soil prop-
erties, the treatment method, and parameters investigated in this
study.
• The effect of thermal treatment on excavation soil depends on
the minerology and physical properties of the clay minerals
present in them. From TGA, it can be observed that dehydra-
tion occurs at 100°C for MP and HP soil, followed by dehy-
droxylation of Kaolinite at 400°C–600°C, montmorillonite at
600°C–800°C, and illite at temperatures higher than 800°C.
• Treatment temperature has a major influence on almost all prop-
erties of mortar with thermally treated soils. Mortar with MP
soil shows comparatively less property enhancement due to the
presence of illite/stilbite clay, which needs a treatment tempera-
ture well above 1,000°C, whereas mortar with HP soil shows
better results at treatment temperatures ranging from 800°C to
1,000°C.
• In cement mortar with thermally treated (800°C for 90 min) ex-
cavation soil with high clay content (25% to 40%), the percen-
tage reduction in water demand was 68%, due to the growth of
clay-sized particles by sintering. The shrinkage strain of mortar
with HP soil decreased by 96% and strength improved to 85%
compared with mortar with raw soil. This behavior of cement
mortar with thermally treated soils is due to pore refinement
and reduced permeable pore volume in the mortar’s hardened
structure.
• Though temperature treatment results in a marginal increase in
embodied energy (10–120 MJ=Mg) compared with conven-
tional fine aggregates, this depends on the type and amount of
clay mineral in the soil. With MP soil, the embodied energy is
100 MJ=Mg lower than that of the crushed stone aggregate.
Hence, thermal treatment has to be carefully chosen for suitable
materials based on their specific heat capacity.

Appendix I. Response Surface Model Equations for Mortar

Mortar property Response model R2 F-value P-value

MP soil
Water content (kg=m3 ) 907.80592 − ð0.39613 × AÞ − ð0.59622 × BÞ − ð0.000727273 × A × BÞ − 0.9707 46.31 <0.0001
ð0.0000182099 × A2 Þ þ ð0.00375574 × B2 Þ
Dry density (kg=m3 ) 1137.42403 þ ð1.2145 × AÞ þ ð1.86739 × BÞ þ ð0.00190545 × A × BÞ − 0.9506 26.95 0.0002
ð0.000705099 × A2 Þ − ð0.011268 × B2 Þ
Compressive strength (MPa) −5.1275 þ ð0.060967 × AÞ þ ð0.076691 × BÞ þ ð0.0000642424 × A × BÞ − 0.9668 40.75 <0.0001
ð0.0000392778 × A2 Þ − ð0.000441322 × B2 Þ
Drying shrinkage (μstrain) 21816.90097 − ð48.64763 × AÞ − ð27.7264 × BÞ − ð0.0153 × A × BÞ þ 0.9281 18.08 0.0007
ð0.030791 × A2 Þ þ ð0.17787 × B2 Þ
Permeable pore volume (%) 57.05337 − ð0.056118 × AÞ − ð0.10276 × BÞ − ð0.0000538721 × A × BÞ þ 0.9444 23.77 0.0003
ð0.0000253086 × A2 Þ þ ð0.000532599 × B2 Þ
HP soil
Water content (kg=m3 ) 1519.04593 − ð1.5229 × AÞ − ð2.43772 × BÞ − ð0.000215488 × A × BÞ þ 0.9737 51.82 <0.0001
ð0.000483951 × A2 Þ þ ð0.00940312 × B2 Þ
Dry density (kg=m3 ) 633.22158 þ ð2.29589 × AÞ þ ð4.07401 × BÞ þ ð0.00209455 × A × BÞ − 0.9824 78.36 <0.0001
ð0.00136531 × A2 Þ − ð0.020266 × B2 Þ
Compressive strength (MPa) −3.27457 þ ð0.042357 × AÞ þ ð0.078419 × BÞ þ ð0.000119192 × A × BÞ − 0.9631 36.51 <0.0001
ð0.0000154074 × A2 Þ − ð0.000368044 × B2 Þ

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J. Mater. Civ. Eng., 2019, 31(8): 04019137

 Appendix I. (Continued.)
Mortar property Response model R2 F-value P-value
Drying shrinkage (μstrain) 31681.54612 − ð68.33879 × AÞ − ð41.74744 × BÞ þ ð0.014074 × A × BÞ þ 0.9727 49.83 <0.0001
ð0.040299 × A2 Þ þ ð0.097502 × B2 Þ
Permeable pore volume (%) 80.74274 − ð0.070478 × AÞ − ð0.18191 × BÞ − ð0.000040404 × A × BÞ þ 0.9629 36.20 <0.0001
ð0.0000203704 × A2 Þ þ ð0.000606061 × B2 Þ
Note: A = temperature; and B = duration.

Appendix II. ANOVA for Mortar Properties

Main effects Interaction effects Quadratic effects
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Response A (°C) B (min) AB A2 B2

MP soil
Water content (kg=m3 ) F-value 226.99 2.24 0.86 0.03 1.34
P-value <0.0001 0.1782 0.3843 0.872 0.2846
Dry density (kg=m3 ) F-value 113.12 5.02 1.79 12.69 3.66
P-value <0.0001 0.0599 0.2227 0.0092 0.0973
Compressive strength (MPa) F-value 156.57 6.15 1.9 36.84 5.25
P-value <0.0001 0.0522 0.21 0.0005 0.0556
Drying shrinkage (μstrain) F-value 68.58 0.02 0.1 21.63 0.82
P-value <0.0001 0.8957 0.7574 0.0023 0.3966
Permeable pore volume (%) F-value 108.46 2.64 0.48 5.44 2.72
P-value <0.0001 0.1483 0.5123 0.0524 0.143
HP soil
Water content (kg=m3 ) F-value 248.42 4.26 0.02 5.01 2.14
P-value <0.0001 0.0779 0.8937 0.0603 0.1874
Dry density (kg=m3 ) F-value 300.6 47.46 0.3 37.35 10.55
P-value <0.0001 0.0002 0.6024 0.0005 0.0141
Compressive strength (MPa) F-value 156.33 19.98 2.76 2.38 1.54
P-value <0.0001 0.0029 0.1409 0.1666 0.2551
Drying shrinkage (μstrain) F-value 192.39 2.84 0.13 53.68 0.35
P-value <0.0001 0.136 0.7325 0.0002 0.5701
Permeable pore volume (%) F-value 162.52 14.92 0.17 2.19 2.19
P-value <0.0001 0.0062 0.6951 0.182 0.182
Note: A = temperature; and B = duration.

References contaminated marine sediments as fine aggregates in cemented mortars.”

ASTM. 2015. Standard test method for flow of hydraulic cement mortar.
ASTM C1437. West Conshohocken, PA: ASTM.
ASTM. 2017a. Standard practice for classification of soils for engineering
purposes (unified soil classification system). ASTM D2487. West
Conshohocken, PA: ASTM.
ASTM. 2017b. Standard test method for bulk density (“unit weight”) and
voids in aggregate. ASTM C29. West Conshohocken, PA: ASTM.
ASTM. 2017c. Standard test method for particle-size distribution
(gradation) of fine-grained soils using the sedimentation (hydrometer)
analysis. ASTM D7928. West Conshohocken, PA: ASTM.
Bhatnagar, J. M., and R. K. Goel. 2002. “Thermal changes in clay products
from alluvial deposits of the Indo-Gangetic plains.” Constr. Build. Mater.
16 (2): 113–122. https://doi.org/10.1016/S0950-0618(01)00031-9.
BIS (Bureau of Indian Standards). 2013. Ordinary portland cement,
53-grade: Specification. IS 12269. New Delhi, India: BIS.
Brooks, R., F. F. Udoeyo, and K. V. Takkalapelli. 2011. “Geotechnical
properties of problem soils stabilized with fly ash and limestone dust
in Philadelphia.” J. Mater. Civ. Eng. 23 (5): 711–716. https://doi.org/10
.1061/(ASCE)MT.1943-5533.0000214.
Cepuritis, R., and E. Mørtsell. 2016. “Possibilities of improving crushed
sand performance in fresh concrete by washing: A case study.” Mater.
Struct. 49 (12): 5131–5146. https://doi.org/10.1617/s11527-016-0849-x.
Couvidat, J., M. Benzaazoua, V. Chatain, A. Bouamrane, and H.
Bouzahzah. 2016. “Feasibility of the reuse of total and processed
Constr. Build. Mater. 112 (Jun): 892–902. https://doi.org/10.1016/j
.conbuildmat.2016.02.186.
da Rocha, C. G., A. Passuello, N. C. Consoli, R. A. Quiñónez Samaniego,
and N. M. Kanazawa. 2016. “Life cycle assessment for soil stabilization
dosages: A study for the Paraguayan Chaco.” J. Clean. Prod. 139 (Dec):
309–318. https://doi.org/10.1016/j.jclepro.2016.07.219.
EEP (Energy and Environmental Profile). 2013. “Energy and environmen-
tal profile of the U.S. mining industry.” Accessed March 4, 2018.
https://www.energy.gov/sites/prod/files/2013/11/f4/stone.pdf.
Egan, G., A. Kumar, N. Neithalath, and G. Sant. 2017. “Re-examining the
influence of the inclusion characteristics on the drying shrinkage of
cementitious composites.” Constr. Build. Mater. 146 (Aug): 713–722.
https://doi.org/10.1016/j.conbuildmat.2017.04.048.
Eid, J. 2017. “New construction material based on raw earth: Cracking
mechanisms, corrosion phenomena and physico-chemical interactions.”
Eur. J. Environ. Civ. Eng. 22 (12): 1–16. https://doi.org/10.1080
/19648189.2017.1373707.
Fernandez, R., F. Martirena, and K. L. Scrivener. 2011. “The origin
of the pozzolanic activity of calcined clay minerals: A comparison
between kaolinite, illite and montmorillonite.” Cem. Concr. Res. 41 (1):
113–122. https://doi.org/10.1016/j.cemconres.2010.09.013.
ICSD. 2009. Inorganic crystal structure database. Germany: FIZ Karlsruhe.
Joshi, R. C., G. Achari, D. Horsefield, and T. S. Nagaraj. 1994. “Effect
of heat treatment on strength of clays.” Appl. Clay Sci. 120 (6):
1080–1088. https://doi.org/10.1016/j.clay.2012.09.010.

© ASCE 04019137-10 J. Mater. Civ. Eng.

J. Mater. Civ. Eng., 2019, 31(8): 04019137

 Khouadjia, M. L. K., B. Mezghiche, and M. Drissi. 2015. “Experimental
evaluation of workability and compressive strength of concrete with
several local sand and mineral additions.” Constr. Build. Mater.
98 (Nov): 194–203. https://doi.org/10.1016/j.conbuildmat.2015.08.081.
Landfield, A. H., and V. Karra. 2000. “Life cycle assessment of a rock
crusher.” Resour. Conserv. Recycl. 28 (3–4): 207–217. https://doi.org
/10.1016/S0921-3449(99)00045-2.
Litvinov, I. M. 1960. Stabilization of settling and weak clayey soils by
thermal treatment. Highway Research Board Special Rep. No. 60.
Washington, DC: National Research Council.
Montgomery, C. D. 2012. Design and analysis of experiments. 9th ed.
New York: Wiley.
Ozer-Erdogan, P., H. M. Basar, I. Erden, and L. Tolun. 2016. “Beneficial
use of marine dredged materials as a fine aggregate in ready-mixed
Downloaded from ascelibrary.org by Nottingham Trent University on 05/23/19. Copyright ASCE. For personal use only; all rights reserved.
concrete: Turkey example.” Constr. Build. Mater. 124 (Oct): 690–704.
https://doi.org/10.1016/j.conbuildmat.2016.07.144.
Priyadharshini, P., K. Ramamurthy, and R. G. Robinson. 2018a. “Reuse
potential of stabilized excavation soil as fine aggregate in cement
mortar.” Constr. Build. Mater., 192 (Dec): 141–152. https://doi.org/10
.1016/j.conbuildmat.2018.10.141.
Priyadharshini, P., K. Ramamurthy, and R. G. Robinson. 2018b. “Sustain-
able reuse of excavation soil in cementitious composites.” J. Clean. Prod.
176 (Mar): 999–1011. https://doi.org/10.1016/j.jclepro.2017.11.256.
Purushothaman, R., R. R. Amirthavalli, and L. Karan. 2015. “Influence of
treatment methods on the strength and performance characteristics of
recycled aggregate concrete.” J. Mater. Civ. Eng., 27 (5): 04014168.
https://doi.org/10.1061/(ASCE)MT.1943-5533.0001128.
© ASCE 04019137-11
J. Mater. Civ. Eng., 2019, 31(8): 04019137
Reddy, B. V. V., and K. S. Jagadish. 2003. “Embodied energy of common
and alternative building materials and technologies.” Energy Build.
35 (2): 129–137. https://doi.org/10.1016/S0378-7788(01)00141-4.
Sannier, L., D. Levacher, and M. Jourdan. 2009. “Economical approach and
validation of treatment methods using binders of contaminated marine
sediments.” Revue Paralia 2: s2.17–s2.32. https://doi.org/10.5150
/revue-paralia.2009.s02.
Sarikaya, Y., M. Onal, B. Baran, and T. Alemdaroglu. 2000. “The effect
of thermal treatment on some of the physicochemical properties of a
bentonite.” Clay. Clay. Miner. 48 (5): 557–562. https://doi.org/10.1346
/CCMN.2000.0480508.
Wang, M. C., J. M. Benway, and A. M. Arayssi. 1990. The effect of heating
on engineering properties of clays. Physico-Chemical Aspects of
Soil and Related Materials Vol. STP 1095. West Conshohocken, PA:
ASTM.
Wang, M. C., M. Jao, and M. S. Ghazal. 2008. “Heating effect on swelling
behaviour of expansive soils.” Geomechan. Geoengin. 3 (2): 121–127.
https://doi.org/10.1080/17486020802069067.
Warshaw, C. M., P. E. Rosenberg, and R. Roy. 1960. “Changes effected
in layer silicates by heating below 550°C.” Clay Miner. Bull. 4 (23):
113–126. https://doi.org/10.1180/claymin.1960.004.23.01.
Yilmaz, G. 2003. “Temperature effects and shrinkage properties on clays.”
Am. Ceram. Soc. Bull. 82 (12): 9601–9605.
Zhang, M. H., and O. E. Gjørv. 1990. “Pozzolanic reactivity of lightweight
aggregates.” Cem. Concr. Res. 20 (6): 884–890. https://doi.org/10.1016
/0008-8846(90)90050-8.
J. Mater. Civ. Eng.