Applied Clay Science 141 (2017) 146–156

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Applied Clay Science

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Research paper

Strength behavior and microstructural characteristics of soft clay

stabilized with cement kiln dust and fly ash residue
Naphol Yoobanpot a, Pitthaya Jamsawang a,⁎, Suksun Horpibulsuk b
a
Soil Engineering Research Center, Department of Civil Engineering, King Mongkut's University of Technology North Bangkok, Thailand
b
School of Civil Engineering and Center of Excellence in Innovation for Sustainable Infrastructure Development, Suranaree University of Technology, Thailand

a r t i c l e i n f o a b s t r a c t

Article history: This study presents the use of cement kiln dust (CKD) and fly ash (FA) to improve the unconfined compressive
Received 9 June 2016 strength (UCS) of soft Bangkok clay compared with ordinary Portland cement (OPC). The UCS tests were per-
Received in revised form 22 February 2017 formed after a curing time of 3, 7, 28 and 90 days. An investigation of each reaction product was conducted
Accepted 24 February 2017
using an X-ray diffraction (XRD) technique, and changes in the microstructures of the stabilized clay were ob-
served using a scanning electron microscope (SEM). The test results revealed that a 13% CKD mixture with a par-
Keywords:
tial replacement of 20% FA was suggested as the optimal content ratio to produce a similar long term strength as
Cement that achieved using the 10% content of OPC. The UCS of the stabilized clay increased relative to the formation of
Cement kiln dust the primary reaction product, calcium silicate hydrate (CSH), as analyzed using the XRD. The formation of this
Fly ash product reduced the void space in the clay structure resulting in denser and stronger of stabilized clay to corre-
Soft clay spond with the compressive strength development with time. The change on microstructure of stabilized clay
Clay stabilization due to the hydration products was evidenced by SEM.
© 2017 Elsevier B.V. All rights reserved.

1. Introduction hydrates (CSH), calcium aluminates hydrates (CAH) and lime. The sec-
ondary products resulting from the pozzolanic reaction between lime
Bangkok is located in the Chao-Phraya delta river plain, which is and clay minerals, clay silica and clay alumina were continuously
comprised of a soft deposit of marine clay layer, i.e., “soft Bangkok formed as CSH and CAH after a curing period. As a result of both reaction
clay”. The undesirable properties of soft clay, i.e., low shear strength products, the clay became denser, stronger and harder, which resulted
and high compressibility, can be strengthened for construction pur- in an increase in the treated clay strength after curing (Bell, 1993;
poses using a process of clay improvement techniques. The most popu- Chang et al., 2007; Ouhadi and Yong, 2008). In addition, cement kiln
lar clay improvement technique is deep mixing, which is widely used in dust (CKD) is alternative stabilizer and the mechanism of strength de-
Europe and Asia (Xu et al., 2006; Xing et al., 2009). The deep mixing velopment could also be considered. The CKD is composed of silica, cal-
technique uses a machine in situ to mix the soft clay and stabilizer to cium carbonate, calcium sulfate and calcium oxide (free lime), which
create a clay mixing column to transfer the load to the deep hardened are minor components of sulfates and chlorides. Since free lime contain-
clay layer. The stabilizer commonly used for deep mixing is ordinary ing binder system reacts with water in the clay, CSH gel is formed due to
Portland cement (OPC), whose increased clay strength is well a pozzolanic reaction and the other products including ettringite,
established (Miura et al., 2001; Mohammad and Alipour, 2012; Yang, monosulfate and syngenite phase were generated. Thus, the CKD and
2012). In Thailand, cement is commonly used as a stabilizing agent in their hydration products may lead to strength increase of the stabilized
geotechnical projects because it is a general construction material that clay. Moreover, the combination of CKD and other pozzolanic materials
is locally available and can achieve compressive strength within a such as slag and fly ash could be more potentially results of mechanical
month. properties (Wang et al., 2004; Peethamparan et al., 2008; Chaunsali and
The mechanism of strength development in clay stabilized with ce- Peethamparan, 2010).
ment (clay cement) can be explained. When cement and water is Considering the cost reduction for the deep mixing process, the in-
mixed with clay, primary and secondary reaction products from the hy- dustrial waste of the alternative stabilizer and the cementitious material
dration reaction are formed, which affect the improved clay cement was compared with the waste of the OPC. One interesting type of waste
properties. The primary products are comprised of calcium silicates is CKD, which is generated in the kiln during the cement manufacturing
process. The cement production in Thailand is approximately 30 million
⁎ Corresponding author. tons per year (Thai Cement Manufacturers Association, 2015), and
E-mail address: [email protected] (P. Jamsawang). roughly 15–20% becomes CKD (EPA U.S. Environmental Protection

http://dx.doi.org/10.1016/j.clay.2017.02.028
0169-1317/© 2017 Elsevier B.V. All rights reserved.
 N. Yoobanpot et al. / Applied Clay Science 141 (2017) 146–156 147

Agency, 1993; Rahman et al., 2011), which is approximately 4.5–6.0 Table 1

million tons per year. CKD is a fine particle material removed from ce- Geotechnical properties of base clay.

ment kiln by exhaust gases and collected using electrostatic precipitator Properties Standard test method Value
equipment (Najim et al., 2014). Natural water content (%) ASTM D2216-10, 2010 93
Generally, CKD is primarily composed of groups of calcium carbon- Liquid limit (%) ASTM D4318, 2010 88
ate and silicon dioxide, which resemble the cement kiln raw feed but Plastic limit (%) ASTM D4318, 2010 36
vary in the amounts of chloride, alkalis and sulfate (Kunal et al., 2012). Plasticity index (%) ASTM D4318, 2010 52
Liquidity index ASTM D4318, 2010 1.1
The composition of the CKD is highly variable depending on the raw
Clay content (%) ASTM D422-63, 2007 70
material, dust collection method, operation system and type of fuel Activity ASTM D422-63, 2007 0.74
used in each factory (Maslehuddin et al., 2009). Based on the above rea- Wet unit weight (kN/m3) ASTM D7263, 2009 14.9
sons, it is necessary to investigate the CKD before its application in soft Specific gravity ASTM D854-92, 1994 2.66
clay improvement. A few studies revealed that the use of the CKD as a Undrained shear strength (kPa) ASTM D2166/D2166M-16, 2016 4–10
Soil classification (USCS) ASTM D2487-11, 2011 CH
potential clay stabilizer is comparable to that of the OPC, and it can be
used to increase clay strength, reduce permeability and enhance dura-
bility of the clay (Peethamparan et al., 2009; Amadi, 2014; Hashad and
Ei-Mashad, 2014). be transformed into a viscous form to flow like a liquid. The specific
However, the study shows that the OPC and CKD had a significant in- gravity was 2.66, and the undrained shear strengths ranged from 4 to
crease in the clay strength within a month (Sreekrishnavilasam et al., 10 kPa and were obtained from an unconfined compression test. Ac-
2007; Goodary et al., 2012). Several studies suggested that admixing cording to the Unified Clay Classification System (USCS), the clay can
with pozzolanic materials enhanced the long term strength (Kolias et be classified as clay CH with a high plasticity. The chemical composition
al., 2005; Zentar et al., 2012; Chaunsali and Peethamparan, 2013). Fly of the clay was performed using an X-Ray Fluorescence (XRF) analysis,
ash (FA) has long been understood as an industrial waste with pozzola- as indicated in Table 2, to reveal the primary compositions of the clay
nic material properties in a concrete field. Fly ash is the industrial waste to be SiO2, Al2O3 and Fe2O3. The stabilizers used in this study were
by-product created from the coal combustion process in power plants OPC, CKD and FA. The chemical compositions of the stabilizers and the
that has been pulled out of the boiler by flue gases and collected using base clay were determined using the XRF analysis, as indicated in
electrostatic precipitators into a bag. Generally, the primary chemical Table 2. The specific gravity of the OPC Type I was 3.15. The primary
composition of FA are silicon dioxide (SiO2), aluminum oxide (Al2O3) compositions of the commercial OPC Type I were CaO and SiO2 as well
and ferric oxide (Fe2O3), hence it can be regarded as a pozzolanic mate- as Al2O3 and Fe2O3. The particles of the OPC were observed using an
rial (Sezer et al., 2006; Wu et al., 2014). In Thailand, the amount of FA SEM micrograph (Fig.1a), which illustrates that the particles have a
generated from the Mae Moh electric power plant, which is the largest rough surface, sharp corners and are non-uniformly shaped. The CKD
electric power plant, is more than approximately 3.2 million tons per was obtained from the cement factory, which is located in the Saraburi
year (Electricity Generating Authority of Thailand, 2015). Using FA province of Thailand. The compositions of the CKD consist primarily of
would be beneficial for several environmental reasons, such as relieving CaO and SiO2 with Al2O3 and Fe2O3, which are similar to those found
air pollution, reducing the amount of leachate from FA during storage to in the OPC. The CaO and SiO2 contents in the CKD are lower than that
seep through the underground water layer and saving natural resources in the OPC. The specific gravity of the CKD was 2.73, and the fineness
when using FA as a replacement for raw materials used in cement ranged between 3000 and 3400 cm2/g. Fig. 1b illustrates the SEM micro-
manufacturing process. An increased use of the FA as a partial cement graph of the CKD particles, which revealed that the particles of the CDK
replacement not only adds value of such industrial waste but also pre- were similar to that of the OPC in terms of roughness and sharpness.
sents cost savings in construction projects. A few researchers presented The FA used in this study was supplied from the Mae Moh electric
that the FA can be applied in geotechnical projects to enhance clay power plant, which is located in the Lamphang province of Thailand.
strength, increase bearing capacity, reduce swell potential of expansive The chemical composition of the FA consists of high SiO2 contents
clay, and maintain low permeability of the stabilized clay (Singh et al., with Al2O3, Fe2O3 and CaO. According to the ASTM standard (ASTM
2008; Jongpradist et al., 2010; Kogbara et al., 2013; Voottipruex and C618-12a, 2012), FA is classified as a class C for pozzolanic material
Jamsawang, 2014). These studies recommended that a suitable amount properties, for which the composition summations of
of FA should be considered before use due to the variations in its prop- SiO2 + Al2O3 + Fe2O3 are between 50% and 70% by dry weight. The spe-
erties at different areas. cific gravity of the FA was 2.53, and the fineness ranged between 3200
The primary objective of the current study is to determine the and 3600 cm2/g. The SEM micrograph (Fig. 1c) indicated that most of
strength of the stabilized clay using cementitious materials as stabi- the particle shapes of FA were spherical.
lizers, such as OPC and CKD, and partially replacing the CKD with pozzo- The grain size distribution (GSD) curves for the OPC, CKD and FA
lanic material using FA. Based on a compressive strength test, the were obtained using laser particle size analysis, and the GSD curves
increase in strength of the treated clay was compared with the reaction for the soft clay were obtained using a hydrometer analysis (ASTM
products from the hydration process, which were investigated using an D422-63, 2007). These curves are plotted together for comparison, as
X-ray diffraction (XRD) analysis. The changes in the stabilized clay shown in Fig. 2. The GSD curves for the OPC, CKD and FA were similar
structure were observed using a scanning electron microscope (SEM).

Table 2
2. Experimental program Chemical composition of base clay, OPC, CKD and FA.

2.1. Materials Compound Base clay OPC CKD FA

Silicon dioxide (SiO2) 61.17 18.43 14.94 37.34

The typical soft Bangkok clay was used as the base clay in this study. Alumina oxide (Al2O3) 21.64 4.95 4.07 18.63
Ferric oxide (Fe2O3) 9.32 3.29 2.27 13.17
The clay sample was collected from a depth of 2–6 m at a construction
Calcium oxide (CaO) 1.03 66.35 53.89 17.85
site near Bangkok, Thailand. The geotechnical properties of the base Magnesium oxide (MgO) 1.68 0.86 1.84 3.92
clay were determined by the ASTM Standard Test Methods and are Sulfur trioxide (SO3) 1.15 3.18 10.96 3.51
summarized in Table 1. The natural water content was 93%, and the liq- Potassium oxide (K2O) 2.53 1.22 3.62 2.98
uid limit and the plastic limit was 88% and 36%, respectively, which cor- Na2O + TiO2 + other 0.57 0.15 2.78 1.96
Loss on ignition (% by mass) 0.91 1.57 5.63 0.64
responds to a liquidity index of 1.1. Thus, this clay, when remolded, can
148 N. Yoobanpot et al. / Applied Clay Science 141 (2017) 146–156

Fig. 2. GSD curves for base clay, OPC, CKD and FA.

Japan International Cooperation Agency, 1998), the optimum OPC con-

tents generally used in the soft Bangkok clay improvement application
range from 80 to 200 kg/m3 of wet clay volume, and the water-cement
(W/C) ratios range from 0.8 to 1.2. For example, the high cement con-
tents of 150–200 kg/m3 are frequently used for DCM column applica-
tions due to the quality control of the clay-cement mixture (Lai et al.,
2006; Horpibulsuk et al., 2011a, 2012a,b; Jamsawang et al., 2011,
2015; Voottipruex et al., 2011a,b). Therefore, in this study, cement con-
tents of 150 and 200 kg/m3 of wet clay volume, which correspond to
10% and 13% of dry clay weight, respectively, were selected, and a partial
replacement of the CKD with10% and 20% FA by dry weight was applied
to produce various clay-cement mixtures. The W/B ratio of 0.8 was fixed
throughout the experimental program. The details of all the mixture
proportions are listed in Table 3.

2.3. Unconfined compressive strength test

The specimen preparation for the unconfined compressive strength

(UCS) test was performed in accordance with the JGS standard using the
non-compacted method (JGS T821–1990, 1990). The specimens were
prepared by pushing the homogeneous clay-cement mixture into a cy-
lindrical mold (50-mm diameter and 100-mm long) and curing for 24 h.
After 24 h, the specimens were de-molding and immediately wrapped
with a tight plastic sheet to prevent losing moisture content from the
specimen surfaces and cured for 3, 7, 28 and 90 days. The UCS tests
were performed after the required curing time was reached. The aver-
age UCS was obtained from the test results of three samples.

2.4. XRD and SEM analyses

An XRD analysis was performed to investigate the reaction products

of the stabilized clay. Furthermore, this method was used to examine
the correlation between the UCS and the intensity of the reaction prod-
uct from the hydration reaction process, which was conducted on the
Fig. 1. SEM micrographs for: (a) OPC, (b) CKD and (c) FA. failure plan of the specimen after the UCS test. A SEM analysis was

while the particle sizes of the soft clay were much smaller than those of Table 3
OPC, CKD and FA. The average of D50 (the diameter at which 50% of the Mixture proportion.
particles have a smaller diameter) of the OPC, CKD and FA were Cementitious
0.01 mm. The base clay is dominated by the clay content with a clay content (%)
Replacement of CKD by FA
size fraction of 70%, which corresponds to an activity of 0.74.
Sample OPC CKD (by dry weight), %

C10 (reference) 10 – –
2.2. Mixture proportions
K10 – 10 –
K10FA10 – 10 10
To improve the UCS of the soft Bangkok clay, the base clay was K10FA20 – 10 20
mixed with the OPC and CKD stabilizers, and the CKD was partially re- K13 – 13 –
placed by the FA. Based on the recommendation from a joint study per- K13FA10 – 13 10
K13FA20 – 13 20
formed in Thailand and Japan (Department of Highways of Thailand and
 N. Yoobanpot et al. / Applied Clay Science 141 (2017) 146–156 149

used to further investigate the changes in the microstructure of the sta- increased at 90 days, which was similar to the strength characteristics
bilized clay. After the UCS test, a SEM was used to observe with the same of the C10 and K10 mixtures (no FA content). Once the CKD was partial-
failure plans of the samples those investigated using the XRD analysis. ly replaced by 10% FA, the short term strength of K13FA10 increased
with time but at a relatively lower rate than that of K13. At 90 days, a
3. Results and discussions slightly greater strength than that of K13 was observed. After adding a
20% replacement of FA, the strength of K13FA20 increased with time;
3.1. Strength development of the stabilized clay however, it was lower than those of K13 and K13FA10 at 3, 7 and
28 days. At 90 days, the strength of K13 and K13FA10 was 9% and 19%,
The UCSs for C10 at a curing time of 3, 7, 14, 28 and 90 days were respectively. It can be observed that the short term strength increased
used as a reference to determine the effectiveness of both pozzolanic rapidly when the CKD content increased while the long term strength
materials (CKD and FA) in this study. Fig. 3 presents the strength devel- tended to increase with an increase in the FA content. The strength de-
opment for all of the stabilized clay specimens. The results reveal that velopment curves have the same characteristic curve as the 10% CKD
the strengths of the stabilized clay for all of the mixtures increased mixture but with relatively higher strength. K13FA20 exhibits a yield
with curing time, which was expected. The reference UCSs for C10 ex- strength that is higher than the C10 reference strength at 90 days of cur-
hibited the greatest strengths within a month compared to the other ing time. Thus, K13FA20 is suggested for the optimum content used in
mixtures. The UCS of C10 was found to be 317 kPa at 3 days and in- this study. Based on the compressive strength test results, it is observed
creased rapidly to 508 kPa and 837 kPa at 7 and 28 days, respectively. that the CKD has the potential to be used as a cementitious material to
The UCS slightly increased to 915 kPa at 90 days. It is observed that enhance the stabilized clay strength. Based on the strength develop-
the strength characteristics of C10 rapidly increase in the short term, ment characteristic curve, the mixture contents of only OPC and CKD
i.e., 3 days and 7 days, continuously increase at 28 days, and slightly in- have a significant effect on increasing the short term strength of the sta-
crease in the long term, i.e., 90 days. bilized clay while those with the FA take a major responsibility to in-
The UCSs for K10 were 265, 398, 675 and 706 kPa for curing days of crease in strength in the long term.
3, 7, 28 and 90, respectively. The UCS developments for K10 and C10 Fig. 4a presents the UCS of the stabilized clay for the CKD and the
were similar. However, the UCSs of K10 were significantly lower than CKD partially replaced with FA at 3 days and 28 days. Similar results
that of C10. After the partial replacement of the 10% CKD by 10% FA from previous studies are also plotted together to compare the strength
(K10FA10), the UCS also progressively increased with curing time. At characteristic of the new material and other stabilized clays with differ-
3, 7 and 28 days, the short term strengths rapidly increased; they ent pozzolanic materials. The correlation of the UCSs at 3 and 28 days
were lower than that of K10 but slightly higher in the long term, i.e., was determined using a fitting curve as a linear regression equation as
90 days. When the CKD was replaced by 20% FA, the UCS of K10FA20 follows:
still increased with time. The short term UCSs at 3, 7 and 28 days were
relatively lower than those of K10 and K10FA10. Additionally, the UCS UCS3d ¼ 0:398UCS28d for cement and pozzolan stabilized clay ð1Þ
of K10FA20 at 90 days was slightly higher than those of K10 and
K10FA10 by approximately 3% and 4%, respectively. From the strength UCS3d ¼ 0:376UCS28d for CKD and FA stabilized clay ð2Þ
development characteristic curve, it can be observed that the short
term strengths of the stabilized clay tend to decrease with decreasing Eq. (1) indicates that the UCS of the cement and the pozzolan stabi-
CKD content (increase in FA content) while the long term strengths in- lized clay at 3 days is approximately 0.398 times the UCS at 28 days. For
crease with increasing FA content. However, the UCSs of the stabilized the CKD and the FA stabilized clay, the 3-day strength is approximately
clay with CKD-only and CKD substituted partially with FA are lower 0.376 times that of the UCS at 28 days, as indicated in Eq. (2). It is re-
than that of the OPC stabilized clay for all curing times. vealed that the strength of the CKD and FA stabilized clay in this study
For a higher content of the 13% CKD mixture, the strength of the is slightly less than that of common cement and pozzolan stabilized
CKD-only for K13 was increased to 298, 453, 754 and 772 kPa at 3, 7, clay in the early stages of curing. In a similar analysis, the UCS of the
28 and 90 days of curing, respectively. The strength of K13 rapidly in- CKD and the CKD with FA stabilized clay at 7 days and 28 days curing
creased at 3 and 7 days, continuously increased at 28 days and slightly is compared with the different stabilized clay with cement and pozzola-
nic materials, as illustrated in Fig. 4b. The curve fitting by linear regres-
sion equation for the strength at 7 days and 28 days can be given as
follows:

UCS7d ¼ 0:626UCS28d Cement and pozzolan stabilized clay ð3Þ

UCS7d ¼ 0:587UCS28d CKD and FA stabilized clay ð4Þ

Eq. (3) indicates that the UCS of the cement and the pozzolan stabi-
lized clay at 7 days is approximately 0.626 times the UCS at 28 days, and
Eq. (4) indicates that the 7-day strength of the CKD and the FA stabilized
clay is approximately 0.587 times the UCS at 28 days. It is indicated that
the increase in the strength of the CKD and FA stabilized clay is slightly
lower than that of common cement and pozzolan stabilized clay within
a week of curing. Additionally, Horpibulsuk et al. (2011b) present the
general theory equation for the strength development of cement
admixed with soft Bangkok clay in Eq. (5) as follows:

UCSd =UCS28d ¼ 0:026 þ 0:293 ln ðdÞ ð5Þ

Here UCSd is the strength after curing for d days; UCS28d is the strength
at 28 curing days; and d is the curing time in days. This equation is suit-
able because hydration is the primary chemical reaction while the poz-
Fig. 3. Strength development for all of the stabilized clay specimens. zolanic reaction is minor. Fig. 4c depicts the strength development
150 N. Yoobanpot et al. / Applied Clay Science 141 (2017) 146–156

equation of the CKD and the FA stabilized clay compared with the above
theory. It is observed that the study equation is close to the theory equa-
tion for cement admixed with soft Bangkok clay, and the general equa-
tion in this study can be expressed in Eq. (6) as follows:

UCSd =UCS28d ¼ 0:133 þ 0:237 ln ðdÞ ð6Þ

The development characteristic curve of modulus of elasticity (E50),

as indicated in Fig. 5, has a similar trend to the strength development
curve. The reference C10 achieves the highest modulus within a
month as compared to the other mixtures. It is shown that the modulus
of C10 rapidly increased within a week, continued to increase at 28 days,
and then slightly increased at 90 days of long term curing. Considering a
10% CKD mixture content, the modulus of K10 rapidly increased at 3 and
7 days. At 28 days, E50 continuously increased and then slightly in-
creased at 90 days. The development curve modulus of K10 has a similar
trend to that of C10 but a relative lower content. After partially replacing
CKD by 10% FA, E50 also increased with curing time. The short term
modulus at 3, 7 and 28 days increased less than that of K10 but had a
slightly greater modulus at 90 days. When the FA replacement was in-
creased to 20%, the modulus of K10FA20 also increased with time. At
3, 7 and 28 days, E50 is relatively less than those of K10 and K10FA10
while the long term modulus is slightly higher than those of K10 and
K10FA10 at approximately 11% and 6%, respectively. From the charac-
teristic curve of the E50 development, it can be observed that the short
term modulus tends to decrease with a decrease in the CKD content (in-
crease in FA content) while the long term modulus tends to increase
with an increase in the percentage of FA replacement. However, the
modulus of the stabilized clay using CKD-only and CKD replaced with
FA are lower than that of the OPC stabilized clay for all curing times.
For a 13% CKD content, the E50 of the CKD alone of K13 rapidly in-
creased at 3 and 7 days, continuously increased at 28 days and slightly
increased at 90 days, which is similar to the E50 development curve of
C10 and K10 (no FA content). As a result of the partial replacement of
CKD by 10% FA, the short term modulus of K13FA10 also increased
with curing time but was relatively lower than that of K13. For the
long curing time of 90 days, the E50 was slightly greater than that of
K13. After a 20% replacement of CKD by FA, E50 of K13FA20 increased
with time; however, it was relatively lower than those of K13 and
K13FA10 for a short term curing time. At 90 days, the E50 was greater
than those of K13 and K13FA10 at 28% and 22%, respectively. It can be
observed that the short term E50 increased rapidly when the CKD con-
tent increased while the long term E50 tended to increase with an in-
crease in the FA content. These E50 development curves are similar to

Fig. 4. (a) UCS at 3 and 28 days (b) UCS at 7 and 28 days (c) generally equation for strength
development for stabilized clay specimens. Fig. 5. Development of E50 for all of the stabilized clay specimens.
 N. Yoobanpot et al. / Applied Clay Science 141 (2017) 146–156 151

the characteristic curve of the 10% CKD mixture but have a relatively
higher E50. The relationships of the E50 and the UCS for the different sta-
bilized clay are illustrated in Fig. 6. The ratios of the E50 to the UCS for the
different cement and pozzolanic materials stabilized clay range from ap-
proximately 99–159. The data ratio of the stabilized clay in this study
was also plotted, and it was revealed that a ratio of approximately 114
is within the range for common cement stabilized clay.

3.2. Investigation on reaction products using XRD analysis compared to

strength development

XRD diffractometer measurement was performed to evaluate clay

mineral of untreated base clay and reaction produced after admixed
with stabilizer, OPC, CKD and FA, and then scanned with a 2Theta
value ranging from 2° to 70°. The investigated focusing on the phase
change analysis of the products of stabilized clay compared with the
compressive strength tested with times. For a better characterization
of clay minerals in the base clay sample, the XRD analysis was per-
formed in normal, glycoled and calcined forms (Gapak et al., 2017). In
Fig. 7. Clay mineral identification by X-ray diffraction for base clay in normal, untreated,
the glycoled form, the base clay sample was ethylene glycole solvated glycolated and calcined forms.
in vapors at 60 °C in an incubator for 72 h for identification of clay min-
eral phase. In the calcined form the base clay samples was heated to
600 °C in muffle furnace and then cooled at the room temperature be- seen that the new reflections of calcium silicate hydrate (CSH,
fore carrying out the XRD to predict change in the d001-value of various H6Ca3O10Si2), calcium hydroxide (CH, Ca(OH)2) and ettringite
phyllosilicates. The XRD analysis results, as shown in Fig. 7, present the (Ca6Al2(SO4)3(OH)12·26H2O) phases appeared in stabilized clay. Fur-
non-clay mineral (quartz) and three reflections of clay mineral includ- thermore, the remaining part of the unhydrated reactant formed
ing montmorillonite, illite and kaolinite. The d001-values are tabulated tricalcium silicate (C3S, Ca3SiO5) and dicalcium silicate (C2S, Ca2SiO4)
in Table 4. The basal spacing at reflections for montmorillonite within also were found. The XRD pattern indicated that the reflection of the
the range of d001-values of 12.5 Å (7.07°, 2Theta) to 15 Å (5.89°, CSH intensity increased rapidly at 3 and 7 days, continuously increased
2Theta) exhibits the presence of Na-montmorillonite (d001-value of at 28 days and slightly increased at 90 days, which is agreeable to the
12.5 Å) and the Ca-montmorillonite (d001-value of 14–15 Å) that corre- UCS development curve. The new ettringite reflections also appeared
sponds to the previous studies by Peethamparan et al. (2009) and Al- at 3, 7, 28 and 90 days have trend to increase with time similar to an in-
Mukhtar et al. (2010). After glycolated, d-value was left shift and in- crease of CSH. It is note that ettringite crystal beneficial to enhance con-
creased to 17.95 Å (4.92°, 2Theta). For heating process, the montmoril- crete strength was suggested by previous study (Xu et al., 2012;
lonite reflection decreased and right shift to a maximum d001-value of Scholtzová et al., 2015). The product CH, which has a lower intensity
11 Å (8.04°, 2Theta). The d001-value for illite was 9.96–10.1 Å than that of CSH, tends to slightly increase with time, while the reac-
(8.88° − 8.75°, 2Theta), which is constant after ethylene glycole solvat- tants C3S and C2S slightly decrease with time. It can be seen that the in-
ed and heated at 550 °C. The d001-value for kaolinite was 7.14 Å (12.40°, tensities of C3S and C2S decreased with time due to the increase in the
2Theta) after ethylene glycole solvated. The kaolinite reflections disap- hydration process, thus creating increased amounts of the CSH and CH
peared after heated at 550 °C. products during the curing period (Mendoza et al., 2015). In addition,
For XRD analysis of treated clay, K13FA20 was suggested as the op- it was also observed that the montmorillonite reflection of the base
timal mixture content was selected to compare the reaction products clay decreased after admixed with OPC for 3 days. The reflection reduc-
of the OPC-only and the CKD-only mixture, i.e., C10 and K10. The XRD tion was more pronounced in the case of curing days of 7, 28 and 90. The
patterns of the C10 at 3, 7, 28 and 90 days compared with base clay result of this XRD analysis indicates that the significant reduction of
was presented in Fig. 8a. After cement was added 3 days, it can be montmorillonite reflection had an effect on changing the mineralogy
of the clay as a result of the new major reaction products, CSH and
ettringite were formed (Dafalla and Mutaz, 2012). Due to an increasing
of CSH development with time and ettringite exhibited yield intensity
greater than that of the other products, it is believed that CSH and
ettringite are principally responsible for the strength development of
the stabilized clay. Fig. 9 was presented the development curve of
CSH/Quartz ratio with time which then similar trend as the strength de-
velopment curve.
Fig. 8b presents the XRD pattern of the K10 sample. It is revealed that
the CSH and CH products formed were similar to those found in the C10

Table 4
Value of d001-value of clay minerals by XRD analysis in normal, glycoled and calcined
forms (CuKα-radiation).

Form Montmorillonite Illite Kaolinite

Normal 12.5–15 Å 9.96–10.1 Å 7.14 Å

2θ, 7.07°–5.89° 2θ, 8.88°–8.75° 2θ, 12.40°
Glycoled 17.95 Å 9.96–10.1 Å 7.14 Å
2θ, 4.92° 2θ, 8.88°–8.75° 2θ, 12.40°
Calcined 10.2–11 Å 9.96–10.1 Å Disappear
2θ, 8.67°–8.04° 2θ, 8.88°–8.75°
Fig. 6. Relationships of E50 and UCS for difference stabilized clay specimens.
152 N. Yoobanpot et al. / Applied Clay Science 141 (2017) 146–156

sample whereas the ettringite was not been found. The developments of
the CSH intensity for K10 tend to increase with curing time. It is showed
that the CSH intensity increases rapidly in the short curing period of
3 days and 7 days with a continuous increase at 28 days and slightly in-
creases in the long term, i.e., 90 days. The montmorillonite reflection de-
creased with an increased time, which is similar to C10. It can be

Fig. 9. Development of CSH-Quartz ratios for stabilized clay specimens.

inferred that montmorillonite reacts with CKD to generate CSH. The de-
velopment of the CSH/Quartz ratio has a similar trend to that of the C10
strength development curve but relative lower as showed in Fig. 9. Al-
though K10 has the same content as C10, the CSH product was formed
in smaller amounts due to the effect of the CKD having a lower CaO con-
tent (Table 2), which is an important composition of the raw material
used for the cement hydration process, than that of the cement, as men-
tioned in a previous study (Chew et al., 2004; Ganesan et al., 2008;
Saeed et al., 2014). In addition, non-appeared of ettringite crystal was
effected to low strength when relative compared with cement. Howev-
er, the CKD-only mixture was found to have the same reaction products
as the OPC mixture, which can contribute to the increase in strength in
the stabilized clay. It is indicated that the CKD can be potentially used as
a cementitious material in soft clay improvement.
The XRD pattern of K13FA20 is illustrated in Fig. 8c. The pattern pre-
sents CSH and CH as the primary reaction products, similar to those
found in the C10 and K10 samples. Furthermore, the ettringite was
not found. It was also observed that the montmorillonite reflection re-
duced with increased time. Consideration of the CSH/Quartz ratio, the
lower compared to those of C10 and K10 was presented at 3, 7 and
28 days. For long term curing, i.e., 90 days, CSH/Quartz ratio is higher
than that of K10 and is markedly higher than that of the C10 reference
mixture as showed in Fig. 9. Although ettringite was not been found in
this mixture, the CSH/Quartz ratio were higher than OPC-only and
CKD-only for long time curing. It can be believed that the beneficial of

Fig. 8. X-ray diffraction patterns of stabilized clay specimens: (a) C10, (b) K10 and (c)
K13FA20 at various curing times. Fig. 10. X-ray diffraction patterns for stabilized clay specimens after soaked for 3 days.
 N. Yoobanpot et al. / Applied Clay Science 141 (2017) 146–156 153

the FA, having pozzolanic material properties, has an important effect curing. Due to the rate of increase in the CSH/Quartz ratio having a sim-
on the continuous increase in the amount of reaction products (second- ilar trend as the strength development characteristic curve depicted in
ary reaction product) generated for the long term curing period Fig. 9, it can be concluded that the CKD and OPC have a significant effect
(Moraes et al., 2015). The pozzolanic reaction from the FA was beneficial on the strength development in the short term, and the FA played an
in contributing to a higher CSH/Quartz ratio consequence relative to the important role for the strength development in the long term of cured.
higher stabilized clay strength. The analysis of the CSH formation by Furthermore, soaked specimen of stabilized clay was performed to
XRD was agreeable with the result from the UCS test. evaluate the short term durability properties. After soaked for 3 days,
Based on the XRD analysis result, it was observed that the reaction the UCSs for C10, K10 and K13FA20 were 242, 189 and 185 kPa, which
products of the CKD-only and the CKD partial replacement with FA correspond to 76, 71 and 70% of unsoaked strengths, respectively. The
were similar to those found in the OPC mixture. The OPC-only and the XRD patterns of stabilized base clay after soaked for 3 days are present-
CKD-only mixtures formed amounts of CSH in the short term, which ed in Fig. 10. It was found that the kaolinite reflections for all samples
gradually increased during the long term curing period, while the mix- were 12.40° (2Theta), which had the same degree as the unsoaked sam-
ture with the FA content had a higher CSH/Quartz ratio for long term ples. This is evident that the kaolinite has not been dissolved in short

Fig. 11. SEM micrographs for stabilized clay specimens: (a) C10, (b) K10 and (c) K13FA20 at various curing times.
154 N. Yoobanpot et al. / Applied Clay Science 141 (2017) 146–156

Fig. 11 (continued).

term, which is responsible for non-deterioration of the products of sta- CSH with time effected to bonding of clay which increased in clay
bilized clay (Tan, 2011; Schaetzl and Thompson, 2015). strength at 28 days. For 90 days, growth of CSH was heterogeneous ob-
served to distribution on clay surface consequence increased strength
3.3. Changes in microstructures of stabilized clay using SEM observation with curing period. Similar study was found by Peethamparan et al.
(2008) presented that the hydration products of CKD stabilized clay af-
The microstructure of the clay, which was improved by cementitious fected to increase strength with time. The difference compared of mi-
materials, can be observed by SEM. The technique was performed after crostructure of CKD and OPC stabilized clay was considered. Although
the UCS test was completed to observe the change in the microstructure the use of CKD effected to enhance clay strength, it was due to the ben-
of the stabilized clay. The observation of C10 is depicted in Fig. 11a illus- eficial of only major CSH to fill with pore space creating of clay denser.
trated that the major hydration reaction products of OPC stabilized clay For OPC stabilized clay, not only the CSH fabric fill with pore space be-
are CSH and ettringite, confirmed by XRD analysis, was covered on clay tween clay particles but also intercrossing of ettringite crystals together
surface in the early stages of 3 days and 7 days. The CSH products as pre- with CSH and clay cluster effected to clay denser and stiffer. By above
sented in the fabric form was spread distribution on clay cluster and reason, OPC stabilized clay was significant increased clay strength
filled pore space between clay particles resulting denser in clay struc- than CKD in order to compare with the same amount of stabilizer
ture. The ettringite crystals detected through XRD was also found on content.
clay surface. The needle-like ettringite crystal was formed between A significant change in the clay structure of CKD and fly ash stabi-
clay and CSH fabric consequence in clay packed structure and stiffer. lized clay, K13FA20, is illustrated in Fig. 11c. It was observed that the
The agreeable observed by Bahmani et al. (2016) found that the hydra- main hydration reaction product is CSH which was analyzed by XRD
tion products affecting clay denser and stiffer after cement was applied similar to CKD-only stabilized clay in Fig. 11b. At 3 days, CSH fabric
to soft clay. At 28 days, an additional amount of CSH fabric and ettringite was formed cover with clay surface similar to those found in the C10
crystals was continuously formed over a period of curing to cover the and K10 sample. Furthermore, it was observe that the FA particles
clay surface which makes clay structure stiffer resulting increased in were distributed together with the CSH fabric and filled in the void
clay strength. For long term curing, i.e., 90 days, intercrossing between space between clay particles. This effected to reduce the volume of
clay particle together with CSH and ettringite were continuous formed void in clay structure resulting in overall denser. At 7 days, more
affected to the improved clay structure become stiffer resulting in- amounts formed of CSH fabric affected to make the clay became denser
creased of clay strength with curing time. In addition, Horpibulsuk et with an increased with CSH growth and the continuous forms of CSH
al. (2010) stated that the advantage of continuous growth of hydration fabric were observed at 28 days cured. At 90 days, a significant amount
products was added up the inter-cluster bonding of clay and contain the of CSH fabric was formed to cover both the clay surface and the FA par-
pore space between clay particles. This changed to the volume of pores ticle. At this stage, it was assumed that the abundant CSH fabric along
that smaller than 0.1 μm is reduced resulting in clay strength increased. with the FA particles embedded in the clay structure that became a
It was found that a change on stabilized clay structure was conformed to clay matrix, and the FA particles filled the void space in the clay struc-
XRD analysis result and compressive strength test. ture, which resulted in higher clay strength after curing. The advantage
Change on microstructure of CKD stabilized clay as showed in Fig. used of FA for to cementitious products was suggested as previous stud-
11b. It was found that the major hydration reaction product is CSH ied found that the FA beneficial to reduced void space of clay particle
which was detected by XRD analysis. At the initial stage of 3 days and and enhanced clay strength in long term curing (Wang et al., 2013;
7 days, CSH fabric was formed cover with clay surface and contained Shaheen et al., 2014). Based on the SEM observation, it can be concluded
in pore space of clay particle resulting in clay denser. However, the nee- that the formation and the progressive growth of the primary reaction
dle-like ettringite was not being observed in SEM micrograph which products causing the stabilized clay structure to become stiffer and
conformed to not be found in XRD analysis. The continuous formed of denser than untreated clay, which results in the increase in strength
 N. Yoobanpot et al. / Applied Clay Science 141 (2017) 146–156 155

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land Research Fund under the TRF Senior Research Scholar program lidification of contaminated soil: performance properties and initiation of operating
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