Materials 15 03087
Materials 15 03087
Article
Hydrophobic Effect of Soil Stabilization for a Sustainable
Subgrade Soil Improvement
Ali Muftah Abdussalam Ezreig, Mohd Ashraf Mohamad Ismail * and Khaled Ibrahim Azarroug Ehwailat
School of Civil Engineering, Engineering Campus, Universiti Sains Malaysia, Nibong Tebal,
Seberang Prai Selatan 14300, Pulau Pinang, Malaysia; aliezreig@student.usm.my (A.M.A.E.);
khaledazrog@student.usm.my (K.I.A.E.)
* Correspondence: ceashraf@usm.my
Abstract: The chemical process of using additives to stabilize soils is to improve soil that lacks strong
engineering properties. In particular, the moisture susceptibility of subgrade soil through seasonal
rains is still questionable. The presence of water in the construction is the cause of deterioration
and premature distress of pavements and their supporting geotechnical structures. In this work, the
chemical use of hydrophobic caltite (HC) in various amounts (ranging from 3%, 5%, to 7%) and 5%
of cement to enhance laterite soils is investigated. The investigation includes the evaluation of soil
properties, such as, unconfined compressive strength (UCS) by curing in air and under water, flexural
strength (FS), and California Bearing Ratio (CBR) soaked and unsoaked. The addition of caltite with
cement increases the strength characteristics with the UCS values of 2078–2853 kPa during the early
curing stages (7th day), and 4688–4876 kPa after 90 days of curing. The added caltite in the cement soil
samples shows a reduction index of strength loss underwater with the UCS values of 3196, 3334, and
3751 kPa for caltite cemented soil when compared with cement soil alone. FS results suggest that the
inclusion of caltite in cement means that post-peak behavior can be enhanced, reducing the brittleness
and increasing the ductility. The successful reaction with soil additives occurred in the curing period
of 7 days. In terms of the microstructural analysis, results show that HC with cement reduces the
Citation: Ezreig, A.M.A.; Mohamad
porosity, voids, and cracking of laterite soils. Furthermore, new polymer globules, products from the
Ismail, M.A.; Ehwailat, K.I.A.
reaction, appeared on the clay particle surfaces, thereby reducing the water absorption. The addition
Hydrophobic Effect of Soil
of hydrophobic-caltite to the soil–cement mixture results in increased strength and reduced water
Stabilization for a Sustainable
Subgrade Soil Improvement.
absorption in a soil–cement mix, thus achieving a given strength value.
Materials 2022, 15, 3087. https://
doi.org/10.3390/ma15093087 Keywords: lateritic soil; cement stabilization; caltite; compressive strength; flexural strength; SEM;
California bearing ratio
Academic Editor: Jan Fořt
oxide; (2) presence of a main kaolinite composition of the clay mineral content; (3) a high
reduction in the silica content [5–7].
Almost every tropical and subtropical region with abundant residual lateritic soils
extensively use chemically stabilized soil–cement mixtures. The mixtures can improve
the engineering properties of poor lateritic soils [8,9]. For instance, cement and lime are
extensively utilized in numerous roadbed treatment projects. The benefits include high
levels of integrity and stability and low costs [10,11].
However, although adding cement to soil makes it more robust and stiffer, it also
makes it more brittle. The situation is because every pavement structural layer encounters
tensile or flexural stresses. The effects could be seen on the development of dams, barriers,
or pavements of multiple layers due to the flexure of tensile stress zones in earthen features.
Tensile strength must be considered a critical design feature when embedding reinforcement
materials in soil [12,13]. Some crucial parameters in designing pavements are flexural
strength (FS), unconfined compressive strength (UCS), and soaked California Bearing Ratio
(CBR) [14,15].
However, several tests showed that cement soil is unsuitable for specific projects due to
certain defects, such as low tensile strength, great brittleness, and poor deformability [16,17].
In response to the above-mentioned problems, many researchers have proposed various
improvement methods based on different materials [18–21]. Few studies discovered that
the use of fiber reinforcement technology to enhance mechanical properties effectively
improved the soil [22–25].
Recently, different liquid chemicals, such as sodium silicate, magnesium chloride,
sulfonated oil, canlite, and probase, are used to improve the compressive strength in
road stabilization projects [6,26–30]. Those chemicals are used in unconfined compressive
testing on lateritic soil samples of varying contents. The tests revealed an initial increase in
compressive strength before it decreased with the increase in the sample’s material content.
A necessary supplement to the examination of compressive strength is to assess the tensile
(flexural) of the bound materials. The FS is governed by any failure of the cement-treated
base (CTB) [31].
Some studies indicated that the strength of cement-stabilized lateritic soils is sus-
ceptible to moisture levels even after 28 or 90 days of curing. Given that the stabilized
lateritic soil strength dramatically reduces after water immersion, researchers suggested
that a study on soaked and unsoaked strengths should also be conducted to avoid design
errors [32,33]. To the best of our knowledge, no research has been shown to date on the use
of caltite in pavement geotechnics to improve the durability of cement-stabilized pavement
base/subbase, which is the subject of this study. This study is the first attempt to use caltite
with ordinary Portland cement (OPC), making it novel.
Several experimental studies that examine the feasibility of using local cement-treated
lateritic soil for constructing roads is presented in this study. This study aimed to evaluate
the mechanical behavior of hydrophobic caltite (HC) on the cement soil exposed to water
ingress. A 5% of OPC and various percentages of HC were mixed with lateritic soils.
The preparation involved changing the content of molding water. The soil was subjected
to geotechnical and microscopic tests to determine their initial material characteristics
before adding cement and caltite. Testing involved compaction, unconfined compressive
strength (UCS) in unsoaked and soaked conditions, flexural strength (FS), porosity, and
absorption (PA), California Bearing Ratio (CBR) test, and scanning electron microscopy
(SEM). The outcomes will provide experimental evidence to evaluate the practical usage of
caltite-reinforced cement soil in engineering projects.
Telunjuk, Bandar Baharu, Kedah, Malaysia. The classification of the lateritic soil was tested
following British Standards [34,35], and the results are presented in Table 1. According to
the Unified Soil Classification System (USCS), the soil was classified as silty sand (MS).
Table 1. Physical properties of lateritic soil and caltite used in this study. All units in the soil properties
are in % except *.
2.1.2. HC
Caltite, a unique double-action and a waterproofing compound, could line the pore
and capillary structure of the cement paste, reversing the standard capillary suction and
physically blocking the capillaries when subjected to hydrostatic pressure. The precise
chemical composition of the additive is not in the public domain because as it is a commer-
cially registered brand [36].
2.1.3. OPC
In this study, the OPC conforming to BS EN 197-1:2011 [37] was used to bind the
stabilized soil. The OPC was manufactured by Cement Industries Malaysia Berhad (CIMA).
Care was taken to ensure that the cement did not exceed the 3 month storage period after
production.
2.2. Method
2.2.1. Mix Design
The first soil mixture with 5% cement was prepared, as recommended in previous
studies [38,39]. Next, the second mixture was prepared with different percentages of caltite
Materials 2022, 15, 3087 4 of 17
(5%, 10%, and 15%) before being added to the cement soil mixture. The added cement and
caltite were based on the soil dry weight. In this study, the mechanical tests used were
standard proctor (SP) compaction tests (BS EN 13286-2:2010) [40], UCS tests (BS EN ISO
17892-7:2018) [41], CBR (BS EN 13286-47:2012) [42], and FS tests (ASTM D1635 2019) [43].
All the experimental tests and procedures conducted in this study were based on the British
Standards.
1.600
NLS LS+HC5%
LS+OPC5% LS+OPC5%+HC3%
1.550
LS+OPC5%+HC5% LS+OPC5%+HC7%
Dry Density ( mg/m3 )
1.500
1.450
1.400
1.350
1.300
15.00 18.00 21.00 24.00 27.00 30.00 33.00
Moisture Content (%)
Resultofofthe
Figure1.1.Result
Figure thecompaction
compactiontest
teston
onthe
thelateritic
lateriticsoil
soiland
andcement
cementmixed
mixedwith
withcaltite.
caltite.
4000
CompressiveStrength
4000
3000
3000
Compressive
2000
2000
1000
1000
0
0
7 DAY Unsoaked 28 DAY Unsoaked 90 DAY Unsoaked
7 DAY Unsoaked 28 DAY Unsoaked 90 DAY Unsoaked
Figure 2. Compressive strength for curing in air (7, 28, and 90 days unsoaked).
Figure
Figure 2.
2. Compressive
Compressivestrength
strength for
for curing
curing in
in air
air (7,
(7, 28,
28, and
and 90
90 days
days unsoaked).
unsoaked).
6000
6000
LS+OPC 5% LS+OPC 5% + HC5%
LS+OPC 5% LS+OPC 5% + HC5%
5000
5000
kPa
StrengthkPa
CompressiveStrength
4000
4000
3000
3000
Compressive
2000
2000
1000
1000
0
0
7 DAY soaked 28 DAY soaked 90 DAY soaked
7 DAY soaked 28 DAY soaked 90 DAY soaked
Figure 3. Compressive strength for curing in air (7, 28, and 90 days soaked).
Figure 3. Compressive strength for curing in air (7, 28, and 90 days soaked).
Figure 3. Compressive strength for curing in air (7, 28, and 90 days soaked).
Meanwhile, a smaller rise in UCS was observed when 3% of caltite was added. By
Meanwhile,
contrast, aasmaller
the UCS
Meanwhile, smallerrise
increased in
when
rise inUCS was
wasobserved
5% caltite
UCS when
was added.
observed when 3%
The3% of
ofcaltite
caltitewas
differences added.
added.By
in compressive
was By
contrast,
contrast, the UCS
strength observed increased when
in the soil when
the UCS increased 5%
with the caltite
5%5% was
cement
caltite added.
wasmixture The
added. and differences
The5% in compressive
caltite addition
differences appeared
in compressive
to be the greatest. As previously mentioned, a rise in UCS occurred when the period of
curing continued (Figure 2). However, no significant effect of the caltite solution alone was
observed on the soil.
However, the most significant growth in strength occurred during the initial 7-day
curing period. The combination of treated samples with 5% caltite–cement (LS + OPC +
HC) reached a compressive strength of 2853 kPa after a 7-day curing period compared with
the addition of 5% cement alone (2078 kPa). This pattern represented a value around eight
times higher than the untreated soil strength when 5% of cement was added to the soil and
eleven times when 5% of caltite was added to cement-treated soil.
This strength developed faster during the initial 7-day period than during the sub-
sequent periods (for 28 days, an increment of 230 kPa was observed). The mixture of
However, the most significant growth in strength occurred during the initial 7-day
curing period. The combination of treated samples with 5% caltite–cement (LS + OPC +
HC) reached a compressive strength of 2853 kPa after a 7-day curing period compared
with the addition of 5% cement alone (2078 kPa). This pattern represented a value around
Materials 2022, 15, 3087 eight times higher than the untreated soil strength when 5% of cement was added to7 of the17
soil and eleven times when 5% of caltite was added to cement-treated soil.
This strength developed faster during the initial 7-day period than during the subse-
quent periods (for 28 days, an increment of 230 kPa was observed). The mixture of 5% caltite,
5% caltite, cement, and soil achieved a UCS value of 2853 kPa during the initial 7-day
cement, and soil
curing period (anachieved
increment a UCS
of 753value
kPa),ofwhile
2853 akPa during
final valuethe initialkPa
of 4876 7-day
wascuring
attainedperiod
after
(an increment of 753 kPa), while a final value of 4876 kPa was attained
the 90-day curing (an increment of 188 kPa) compared with the 5% cement soil mixture after the 90-day cur-
ing (an increment
(Figure 2). of 188 kPa) compared with the 5% cement soil mixture (Figure 2).
This
This situation
situation implies
implies that
that most
most reactions
reactions with
with soil
soil stabilizers
stabilizers occurred
occurred during
during the the
initial
initial curing stages. When immersed in water for 24 h and air-dried at least 2hhat
curing stages. When immersed in water for 24 h and air-dried at least 2 at room
room
temperature,
temperature, the the strength
strength of of caltite-cement
caltite-cement soil soil (LS
(LS ++ 5%
5% OPC
OPC ++5% 5%HC)HC)increased
increasedto to3000
3000
and 4235 kPa, respectively, during the 7–28 days with a slight
and 4235 kPa, respectively, during the 7–28 days with a slight strength loss to 4840 strength loss to 4840 kPakPa at
90-day curing periods. By contrast, the cement soil samples (LS
at 90-day curing periods. By contrast, the cement soil samples (LS + 5% OPC) with the + 5% OPC) with the same
conditions reported
same conditions an increased
reported strength
an increased of 2606
strength kPakPa
of 2606 during
during thethe
7-day
7-daycuring
curingperiod.
period.
Meanwhile,
Meanwhile, the strength development decreased to 3429 and 4230 kPa duringthe
the strength development decreased to 3429 and 4230 kPa during thecuring
curing
periods
periodsof of2828andand9090 days.
days.TheThedropdropwaswas
approximately
approximately 9% with the soil
9% with theand soilcement
and cementsam-
ple. By contrast,
sample. By contrast,no decrease
no decrease in strength,
in strength, butbut
rather anan
rather increase,
increase,waswasobserved
observedwith withthe the
cement, caltite, and soil sample (Figure
cement, caltite, and soil sample (Figure 3). 3).
Conversely,
Conversely, the the compressive
compressive strength
strength of of the
the samples
samples treated
treated with
with aacement
cementalone
aloneand and
caltite
caltite liquid additive was reduced when the samples were cured
additive was reduced when the samples were cured 1 day in air and immersed 1 day in air and im-
mersed
in waterinfor water
28 andfor 9028 days
and 90 days under
(curing (curingwater),
under except
water),for except
7 days forof 7 curing
days ofwherein
curing
wherein
an increasean increase
in UCS in UCS2550
until untiland
2550 andkPa
3196 3196ofkPa of mixtures
mixtures was was recorded.
recorded. Meanwhile,
Meanwhile, the
the reduction
reduction ratesrates
in UCSin UCS
at 28at
and2890
and 90 were
days days 3054
wereand3054 andkPa
3206 3206forkPa for the cement
the cement soil
soil samples
samples
(LS + 5%(LS + 5%and
OPC) OPC) andand
3334 3334 andkPa
3751 3751forkPa for caltite–cement
caltite–cement soil+(LS
soil (LS 5%+OPC 5% OPC+ 5%+HC),5%
HC), respectively
respectively (Figure (Figure
4). 4).
6000
LS+OPC 5% LS+OPC 5% + HC5%
5000
Compressive Strength kPa
4000
3000
2000
1000
0
7 DAY 28 DAY 90 DAY
Figure
Figure4.4.Compressive
Compressivestrength
strengthfor
forcuring
curingages
agesof
of 7,
7, 28,
28, and
and 90
90 days
days under
under water.
water.
The reduction in UCS in curing under water caused water ingress to the cement soil
samples. Specifically, cement soil absorbed water in the first 7 days, and the water caused
an increase in the reaction with calcium and in strength in the short term. Thereafter,
calcium was consumed early and led to calcium leaching and a decrease in strength in the
long term.
The compressive strength of the samples treated with a caltite liquid additive showed
more than 5% reduction. According to [27,50,51], the most likely explanation was the
increment of a positive surcharge and soil particle repulsion within the resulting mix. The
chemical stabilizer effect might also explain these outcomes. A small proportion began to
fill the soil voids, thus acting as a cementing bond. Once the chemical stabilizer had filled
each void in this manner, the increased softening state of the mixture that exceeded the
requirement for chemical reaction, resulted in a strength reduction.
The compressive strength of the samples treated with a caltite liquid additive showed
more than 5% reduction. According to [27,50,51], the most likely explanation was the in-
crement of a positive surcharge and soil particle repulsion within the resulting mix. The
chemical stabilizer effect might also explain these outcomes. A small proportion began to
Materials 2022, 15, 3087 fill the soil voids, thus acting as a cementing bond. Once the chemical stabilizer had filled 8 of 17
each void in this manner, the increased softening state of the mixture that exceeded the
requirement for chemical reaction, resulted in a strength reduction.
Furthermore,
Furthermore,the the stabilizer
stabilizer percentage affects clay
percentage affects clayminerals.
minerals.AAsmall
smallcaltite
caltitepercentage
percent-
age was sufficient to produce a clay platelet coating. Nonetheless, an increase
was sufficient to produce a clay platelet coating. Nonetheless, an increase in the stabilizer in the sta-
bilizer percentage in the soil body acts as a lubricant as the clay particles slip
percentage in the soil body acts as a lubricant as the clay particles slip across one another.across one
another. This condition
This condition has reduced has reduced the soil skeleton
the soil skeleton strength.strength.
Therefore,Therefore, in this
in this study, 5%study,
caltite
5%
cancaltite can be considered
be considered as the design
as the optimal optimalfor
design
a soilfor a soil mixture,
mixture, along withalong
thewith the addi-
addition of 5%
tion of 5%
cement tocement
lateritictosoil
lateritic soil for micro-characterization.
for micro-characterization.
3.3.Influence
3.3. InfluenceofofCaltite
CaltiteContent
ContentandandCement
CementononFSFS
Theflexural
The flexuralbehavior
behaviorofofthe
thesoil
soilwas
wassignificantly
significantlyaltered
alteredwhen
whencaltite
caltitewas
wasadded
addedtoto
thespecimen
the specimenwith withcement.
cement.TheThealteration
alterationelevated
elevatedthe
theFS
FSvalue
valuewhile
whilealso
alsoimproving
improvingthethe
stiffness of the specimens. Figure 5 shows a comparison of the flexural loads
stiffness of the specimens. Figure 5 shows a comparison of the flexural loads and deflec- and deflection
curves
tion of the
curves NLS,
of the LS +LS
NLS, HC, LS +LS5%
+ HC, OPC,
+ 5% OPC,andand
LS +
LSOPC
+ OPC+ 5% HCHC
+ 5% mixtures. TheThe
mixtures. host soil
host
(LS) exhibited a frail bending resistance, with values of 178.11, 210.36, and 277.23
soil (LS) exhibited a frail bending resistance, with values of 178.11, 210.36, and 277.23 kPa kPa after
the 7,
after 28,7,and
the 90 days
28, and of curing
90 days periods,
of curing respectively.
periods, respectively.
1800
NLS LS+HC 5% LS+OPC 5% LS+OPC 5% + HC5%
1600
1400
Flexural strength kPa
1200
1000
800
600
400
200
0
7 DAY 28 DAY 90 DAY
Flexuralload–deflection
Figure5.5.Flexural
Figure load–deflectioncurves
curvesofofthe
thetreated
treatedand
anduntreated
untreatedtest
testsamples
samplesafter
after7,7,28,
28,and
and
90 days of curing.
90 days of curing.
Moreover,the
Moreover, thesoil
soilwith
withthe
thecaltite
caltitemixture
mixturealone
alone(LS(LS++5%
5%HC)
HC)hadhadaaweak
weakbending
bending
resistance, measuring only 149.86 and 168.01 kPa. The weak bending resistance
resistance, measuring only 149.86 and 168.01 kPa. The weak bending resistance was most was most
likely due to the lack of calcium hydroxide, which is the basis of the reaction with
likely due to the lack of calcium hydroxide, which is the basis of the reaction with caltite.caltite.
Furtherexplanation
Further explanationwillwillbe
bediscussed
discussedininthe
themicrostructural
microstructuralanalysis.
analysis.
The LS + 5% OPC specimen demonstrated improved bending resistance at 980.30,
The LS + 5% OPC specimen demonstrated improved bending resistance at 980.30,
1334.59, and 1497.73 kPa after the 7-, 28-, and 90-day curing periods. The improvement was
1334.59, and 1497.73 kPa after the 7-, 28-, and 90-day curing periods. The improvement
probably due to the formation of calcium aluminate hydrate (C–A–H) and calcium silicate
was probably due to the formation of calcium aluminate hydrate (C–A–H) and calcium
hydrates (C–S–H) because the cement content was hydrated. This result is consistent with
silicate hydrates (C–S–H) because the cement content was hydrated. This result is con-
previous studies [52].
sistent with previous studies [52].
Meanwhile, the mixture specimens (LS + OPC + 5% HC) exhibited significantly earlier
improved resistance to 1403.43, 1541.7, and 1637.61 kPa after 7, 28, and 90 days of curing
periods, respectively (Figure 5). The trend was substantial due to the reinforcement of 5%
HC, which was introduced during the periods. The 5% HC is a considerable enhancement
in bending resistance and was greater than that observed in the LS + 5% OPC specimens,
as shown in Figure 5.
45
LS+OPC5% LS+OPC5%+HC5%
40
35
30
25
Rate %
20
15
10
0
7 Day 28 Day 90 Day 7 Day 28 Day 90 Day
Figure
Figure6.6.Rate
Rateofofporosity
porosityfor
forcemented
cementedlateritic
lateriticsoil
soilwith
withand
andwithout
withoutcaltite.
caltite.
3.5.Influence
3.5. InfluenceofofCaltite
Caltiteand
andCement
Cementon onCBR
CBR
TheCBR
The CBRisisaameasurement
measurementsystem systemused
usedtotodescribe
describethetheroad
roadsubgrade
subgradestrength.
strength.TheThe
CBR parameter determines the thickness of the pavement and the layers it
CBR parameter determines the thickness of the pavement and the layers it comprises [54]. comprises [54].
Lateriticsoil
Lateritic soilhas
hasCBR
CBR values
values that
that areare relatively
relatively lowlow (<15),
(<15), makingmaking
themthem unsuitable
unsuitable for
for road
road subgrade. The study findings revealed substantial CBR gains (Table
subgrade. The study findings revealed substantial CBR gains (Table 3). A moderate but 3). A moderate
but significant
significant increase
increase in strength
in strength was observed
was observed in theinLS
the LS + OPC
+ OPC and LS and LS + +OPC
+ OPC HC + HC
mix-
mixtures, making the tested soil a suitable material for road construction. The
tures, making the tested soil a suitable material for road construction. The findings of the findings of
the cement-treated soil tests were in line with [49,55]. The use of the mixture (LS + OPC +
cement-treated soil tests were in line with [49,55]. The use of the mixture (LS + OPC + HC)
HC) significantly influenced the CBR rise.
significantly influenced the CBR rise.
Table 3. Summary of the laboratory CBR values.
CBR %
Sample Soil Caltite Cement Curing
Unsoaked Soaked
No. NLS% HC % OPC % Time Day Average %
Top Bottom Top Bottom
NLS 100 0 0 7 11.62 15.56 - - 13.59
LS + HC 100 5 0 7 6.41 8.69 - - 7.55
LS + OPC 95 0 5 7+4 109.5 115.2 93.6 118.5 112.3–106
LS + OPC
95 5 5 7+4 114.1 120.8 110.4 136.2 117.4–123.3
+ HC
When HC with the cement was used, the soil samples showed a noticeable trend for the
CBR to significantly increase over time (Figure 7). Except for the LS + HC mixture, the
CBR value was significantly reduced because this HC had no positive impact in the ab-
sence of cement. The increase in the moisture content was probably because of the rapid
and exothermic nature of the reaction between the soil and the additive, resulting in water
Materials 2022, 15, 3087 loss. However, the soaked CBR samples in water for 4 days, after curing for 7 days,10with of 17
LS + OPC + HC soil mixture yielded higher values than the soaked LS + OPC. The soaked
CBR values for the lateritic stabilized soil are illustrated in Figure 7.
In the case of the unsoaked specimens after the 7-day curing period, the CBR values
Table
ranged3. Summary
from 109% of to
the115%
laboratory
(LS +CBR values.
OPC) and 114% to 120% for the LS + OPC + HC mixture.
When HC with the cement was used, the soil samples showed a noticeable trend for the
CBR %
Soil CBR to Cement
Caltite significantlyCuring
increase over time (Figure 7). Except for the LS + HC mixture, the CBR
Sample No. Unsoaked Soaked
NLS% HCvalue
% was OPC significantly
% Time Day reduced because this HC had no positive impactAverage
in the absence
%
of cement. The increase in theTop moistureBottom
content was Top Bottom
probably because of the rapid and
NLS 100 0exothermic0 nature of 7the reaction11.62between
15.56 - the additive,
the soil and - 13.59
resulting in water
LS + HC 100 5loss. However,
0 the soaked CBR samples in water for 4 days, after curing for 77.55
7 6.41 8.69 - - days, with
LS + OPC 95 0LS + OPC + 5 HC soil 7mixture
+4 109.5 higher
yielded 115.2 93.6the soaked
values than 118.5 LS + OPC.
112.3–106
The soaked
LS + OPC + HC 95 5CBR values5 for the lateritic
7 + 4 stabilized
114.1 soil 120.8
are illustrated
110.4in Figure 7.
136.2 117.4–123.3
160
NLS LS + HC LS + OPC LS + OPC + HC
140
120
100
CBR values (%)
80
60
40
20
0
Top Bottom Top Bottom
Unsoaked Soaked
Figure
Figure7.7.CBR
CBRofof
caltite–cement materials
caltite–cement at a at
materials 7-day curing
a 7-day period
curing with and
period withwithout soakingsoaking
and without under water.
under
water.
4. Discussion of the Effect of HC with Cement on Treated Soil
4. Discussion of the Effect of HC with Cement on Treated Soil
The principal active ingredient in caltite is a soluble ammonium stearate, which ac-
counts The
for principal
30% of its active
weight.ingredient in caltite
Caltite shows is aand
chemical soluble ammonium
physical effects onstearate, which
soil properties
accounts for 30% of its weight. Caltite shows chemical and physical effects
when cement is present, and shows no effect in the absence of cement. The chemical im- on soil properties
when
pact cement
takes is at
place present, and showsstearate
the ammonium no effect in the
stage. absence
This of cement.
situation Thecalcium
produces chemical impact
hydrox-
takes place at the ammonium stearate stage. This situation produces calcium
ide in the soil–cement paste, resulting in the formation of calcium stearate and the release hydroxide
inammonia
of the soil–cement
gas. Somepaste, resulting
studies in thethat
suggested formation
calciumofstearate
calcium stearate and
contributes the improve-
to soil release of
ammonia gas. Some studies suggested
ment and reduces water absorption [56]. that calcium stearate contributes to soil improvement
and reduces water absorption [56].
Consequently, the insides of the capillary pores are coated with a water-repellent
Consequently, the insides of the capillary pores are coated with a water-repellent
membrane, causing capillary suction in the soil to reverse. The caltite physical effect oc-
membrane, causing capillary suction in the soil to reverse. The caltite physical effect occurs
curs during the hardening process. The bleed water moves the suspended microscopically
during the hardening process. The bleed water moves the suspended microscopically
small, asphalted particles (polymer globules) in caltite and collects them in the capillary
small, asphalted particles (polymer globules) in caltite and collects them in the capillary
voids. Figure 8 describes the mechanism of gathering polymer globules. The polymer
voids. Figure 8 describes the mechanism of gathering polymer globules. The polymer
globule mechanism was observed using SEM, as shown in Figure 9. These particles could
globule mechanism was observed using SEM, as shown in Figure 9. These particles could
block the capillaries if the hardened soil is subjected to the ingress of external moisture,
block the capillaries if the hardened soil is subjected to the ingress of external moisture,
especially when the soil meets hydrostatic pressure. This situation happened when the
especially when the soil meets hydrostatic pressure. This situation happened when the
soil is soaked in water for 24 h after drying for at least to 2 h at room temperature before
the UCS test. Subsequently, the soil strength increased more than the dry condition at 7
and 28-day curing times, as shown in Figure 3. This finding is comparable with previously
reported studies in concrete technology [36,57].
Materials 2022, 15, x FOR PEER REVIEW 11 o
Materials 2022, 15, x FOR PEER REVIEW 11 of 17
soil is soaked in water for 24 h after drying for at least to 2 h at room temperature bef
soil is soaked
theinUCS
water forSubsequently,
test. 24 h after drying
the for
soilatstrength
least to increased
2 h at room temperature
more before
than the dry condition
Materials 2022, 15, 3087 the UCS test.andSubsequently,
28-day curingthe soil as
times, strength
shownincreased
in Figure 3.more
Thisthan the is
finding dry condition of
comparable
11 at177 previou
with
and 28-day curing
reported times, as shown
studies in Figure
in concrete 3. This finding
technology [36,57].is comparable with previously
reported studies in concrete technology [36,57].
(a) (b)
(a) (b)
Figure of
Figure 8. Schematic 8. Schematic of thefor
the mechanism mechanism for strength by
strength components components
(a) cementby (a) (b)
and cement and (b) cement–calt
cement–caltite
Figure 8. Schematic of theglobules
by polymer mechanism for strength
gathering components by (a) cement and (b) cement–caltite
by polymer globules gathering in the cracks in thevoid
and cracks and void
cement soil, cement soil,
reinforced byreinforced
caltite. by caltite.
by polymer globules gathering in the cracks and void cement soil, reinforced by caltite.
(a) (b)
(a) (b)
Figure 9. (a,b) SEM images of the soil treated by cement after 28 days of curing period.
Figure9.9. (a,b)
Figure (a,b)SEM
SEMimages
imagesof ofthe
thesoil
soiltreated
treatedby
bycement
cementafter
after28
28days
daysof
ofcuring
curingperiod.
period.
4.1. Microstructural Analysis
4.1.
4.1. Microstructural
MicrostructuralAnalysis
Analysis
The microstructural characterization can provide essential information concern
The
The microstructural
microstructural characterization
characterization can
can provide
provide essential information
essentialprocesses.
information concerning
concerning
the mechanisms that underlie chemical stabilization These include the elem
the
themechanisms
mechanisms that
that underlie
underlie chemical
chemical stabilization
stabilization processes.
processes. These
These include
include the
the element
element
compositions, changes in mineralogy, and the in-filling of vacant pore spaces caused
compositions,
compositions, changes in
changes inBased mineralogy,
mineralogy, and the in-filling of vacant pore spaces caused by
cementation. on the and the in-filling
outcomes of vacant
of the tests used inpore
thisspaces
study,caused by
the optimal HC
cementation.
cementation. Based on the outcomes of the tests used
used in this
this study,
study, the
the optimal
optimal HC
HC and
and
cement levels for all stabilizations were ascertained to be 5%. As a result, the microstr
cement
cementlevels
levelsfor
forall
allstabilizations
stabilizations were
wereascertained
ascertained to be 5%. As aAsresult, the microstructural
tural analysis was aimed to compare 5% to be 5%.
cement with aand
result, the microstruc-
without HC-stabilized later
analysis was aimed
tural analysis to compare
was aimed 5% cement
to compare with and
5% cement withwithout HC-stabilized
and without lateritic.
HC-stabilized lateritic.
4.1.1. 4.1.1. SEM Analysis
4.1.1. SEM
SEM Analysis
Analysis
SEM was
SEM was utilized utilizedthe
to observe to observe the morphologies
morphologies of treated soilof samples
treated soil samples
after after a 28-
a 28-day
SEM was utilized
curing to
period. observe the
Figure that
9a,bthemorphologies
shows of treated soil
that the lateritic–cement samples after a 28-day
mixture changes
underwent
curing period. Figure 9a,b shows lateritic–cement mixture underwent in change
curing period. Figure 9a,b shows
its microstructure thatthat the lateritic–cement
culminated in a denser mixture
structure.underwent
However, changes in
the cement-stabili
its microstructure that culminated in a denser structure. However, the cement-stabilized
its microstructure that
soil micrographculminated in a denser structure. However, the cement-stabilized
soil micrograph showed the showed
presencethe of presence of voids,
voids, porosity, and porosity,
cracking,and cracking,
which which prima
primarily
soil micrograph showedtothe
contributed the presence
loss of of voids,
strength when porosity, and cracking,
underwater. These which
cracks actprimarily
on continuous w
contributed to the loss of strength when underwater. These cracks act on continuous water
contributedingress
to the loss of strength
when the cementwhen soil underwater.
was immersed These
in cracksthis
water; act on continuous was
interpretation waterin agreem
ingress when the cement soil was immersed in water; this interpretation was in agreement
ingress when thethe
with cement soil was
previous immersed
studies [32,58].inMeanwhile,
water; this interpretation
the cement was in agreement
produced a new material w
with the previous studies [32,58]. Meanwhile, the cement produced a new material when
with the previous studies [32,58]. Meanwhile, the cement produced a new material when
treated with a caltite mixture. Hence, the cracked soil structure and porous regions were
filled, as shown in the SEM images in Figure 10a,b.
as formation of gel-like products in the soil microstructure. The alterations had layered the soil
surface. Therefore, the increase in the sample shear strength was due to the contribution of
these new formations.
The formation of polymer globules in the early stages of curing also indicated that
the cement–caltite reaction was rapid. Porosity, voids, and cracking were observed in a
Materials 2022, 15, 3087 12 of 17
soil mixture containing cement. In particular, the new products occupied various porous
parts and micro-cracks in the soil structure.
(a) (b)
Figure10.
Figure 10.(a,b)
(a,b)SEM
SEMimages
imagesof
ofthe
thesoil
soiltreated
treatedby
bycaltite
caltitewith
withcement
cementafter
after28
28days
daysofofcuring
curingperiod.
pe-
riod.
As can be seen in Figure 10a,b, white polymer globules formed inside the soil dur-
4.1.2.
ing theEDX Spectroscopy
28-day curing period. The SEM micrograph revealed that significant alterations
occurred such as formation
Figure 11 and Table 4 of gel-like
show eachproducts in the soil
EDX spectrum formicrostructure. The alterations
the untreated lateritic soil and
had layered the soil surface. Therefore, the increase in the sample shear
the soil with HC and cement additive after compressive strength tests at a curingstrength was due
period
to the contribution of these new formations.
of 28 days. The untreated lateritic soil showed comparably high intensities of Si and Al
peaks,Thewhich
formation of polymer
corresponded to globules in the early
the soil lateritic stages
nature [51].of curing also indicated that the
cement–caltite reaction was rapid. Porosity, voids, and cracking were observed in a soil
mixture containing cement. In particular, the new products occupied various porous parts
and micro-cracks in the soil structure.
Table 4. EDX analysis for untreated and treated lateritic soil after the compressive strength test at a
curing period of 28 days.
Element (wt%)
Mixture Curing
Period (Days) Silicon Aluminum Calcium Iron Carbon Titanium Oxygen Ca/Si
Si/Al
(Si) (Al) (Ca) (Fe) (C) (Ti) (O) Si/Ca
NLS 28 33.02 29.80 – (a) 3.15 27.25 0.66 53.60 – 1.10
LS + OPC 5% 28 40.10 33.40 4.74 10.65 11.11 – 62.83 0.11 8.45 1.20
LS + OPC 5%
28 38.83 24.57 4.47 3.33 28.80 – 64.38 0.12 8.68 1.58
+ HC 5%
Table 4 and Figure 11a–c illustrate how the Si/Al and Si/Ca percentages increased
in the caltite mixed with cement-treated soil compared with the cement-treated soil alone
and the untreated lateritic soil. The reaction between the caltite and the cement caused
an increase, indicating the possibility of a change in the surface particle composition. The
changes resulted from the pozzolanic reaction coating or the production of a new mineral
content in the soil with cement and caltite and cement alone. The hydroxyl group (OH)
was present and increased in percentage due to the reaction between the caltite and cement.
This situation produced new polymer globules, which accumulated in the capillary voids
and prevented water from escaping or evaporating from the soil sample. Next, a pozzolanic
reaction would occur if Ca continued to be available. The reaction would result in the
formation of Ca hydrates because OH, Ca2+ , AlO6 , and SiO4 are present [59,60].
4.1.2. EDX Spectroscopy
Figure 11 and Table 4 show each EDX spectrum for the untreated lateritic soil and
the soil with HC and cement additive after compressive strength tests at a curing period
Materials 2022, 15, 3087 of 28 days. The untreated lateritic soil showed comparably high intensities of Si and
13 ofAl
17
peaks, which corresponded to the soil lateritic nature [51].
(a)
(b)
(c)
Figure
Figure 11.
11. Twenty-eight-day
Twenty-eight-day curing
curing period
period of
of the
the EDX
EDX spectrum
spectrum for:
for: (a)
(a) NLS,
NLS, (b)
(b) LS
LS ++ 5%
5% OPC,
OPC, and
and
(c) LS + OPC + 5% HC.
(c) LS + OPC + 5% HC.
TableAdditionally,
4. EDX analysisthe
for untreated and treated
cementation due tolateritic soil after
the C–A–H andtheC–S–H
compressive strengthreaction
pozzolanic test at a
curing period of 28 days.
depends on the percentage of Si/Al. Increased pozzolans, which are rich in silica and
Curing alumina, contribute to the formation of (wt%)
Element C–A–H and C–S–H. Thus, the formed binder
Mixture Period Silicon unquestionably contributes
Calcium to the higher UCS found in the cement and caltite-modified
Titanium Ca/Si
Aluminum (Al) Iron (Fe) Carbon (C) Oxygen (O) Si/Al
(Days) (Si) (Ca) (Ti) Si/Ca
NLS 28 33.02 29.80 – 3.15 27.25 0.66 53.60 – 1.10
LS + OPC 5% 28 40.10 33.40 4.74 10.65 11.11 – 62.83 0.11 8.45 1.20
LS + OPC 5%
28 38.83 24.57 4.47 3.33 28.80 – 64.38 0.12 8.68 1.58
Materials 2022, 15, 3087 14 of 17
soils compared with the non-treated soil. The process could be explained by the interlocking
arrangement that occurred between soil particles [61,62].
5. Conclusions
Implementing hydrophobic material in cement technology is a crucial feature currently
under development. Hence, the investigation into one method of utilizing HC-cement
treatments to stabilize lateritic soil is vital. A significant discovery of the current study was
that a combinatory action between the cement and caltite overcame stabilization problems.
The following are the summarized concluding details from the laboratory experiments:
• The addition of caltite to soil treated for cement stabilization increases the UCS, shear
strength, FS, and CBR values in the two chemical agents.
• Adding caltite to cement-treated soil improves its post-peak behavior, particularly
during the early curing stages (the 7th day). In this case, the best soil-additive reaction
occurred.
• Stabilizing the soil with reinforced HC resulted in a greater strength than cement
alone, regardless of the curing period. This trend is most noticeable after the 7, 28, and
90 days of curing periods.
• After 7 and 28 days of curing, the soil treated with caltite and cement showed a
significant pozzolanic reaction compared to the soil treated with cement alone or
untreated lateritic soil.
• The interfacial interlocking observed in the soil treated with HC and cement-treated
soil demonstrated effective bonds compared to that with untreated soil. However, the
mixture of HC and cement reduced porosity, voids, and cracking in the soil sample
compared with the cement soil sample.
• SEM and EDX analyses revealed that the reaction that occurs in the soil treated with
caltite and cement mixture resulted in a denser soil. By contrast, the reaction that occurs
in the soil alone tends to result in the binding of soil particles and the strengthening of
soil.
• Finally, the SEM analysis proved that adding caltite to cement soil led to new globular
polymer bonding compounds. These compounds essentially filled the soil cracks and
porous voids. Consequently, the soil density improved with greater strength and more
effective void filling.
In conclusion, adding caltite to cement and soil mixture can significantly strengthen
the treated soil, resulting in suppression of strength loss in cement-treated soil when using
in wet environments. Given that this material is hydrophobic, future research should focus
on improving the soil in other environments.
Author Contributions: A.M.A.E. and K.I.A.E. designed and performed the experimental program;
A.M.A.E. and K.I.A.E. collected and analyzed the experimental data; K.I.A.E. wrote, reviewed, and
edited the manuscript; and M.A.M.I. provided supervision of the manuscript writing. All authors
have read and agreed to the published version of the manuscript.
Funding: This work was funded by the Universiti Sains Malaysia.
Institutional Review Board Statement: Not applicable.
Informed Consent Statement: Not applicable.
Data Availability Statement: Not applicable.
Acknowledgments: The authors would like to acknowledge the Universiti Sains Malaysia for its
financial support.
Conflicts of Interest: The authors declare no conflict of interest.
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