Road Materials and Pavement Design

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Palm oil fuel ash-soft soil geopolymer for subgrade

applications: strength and microstructural
evaluation

Patimapon Sukmak, Gampanart Sukmak, Suksun Horpibulsuk, Monthian

Setkit, Sippakarn Kassawat & Arul Arulrajah

To cite this article: Patimapon Sukmak, Gampanart Sukmak, Suksun Horpibulsuk, Monthian
Setkit, Sippakarn Kassawat & Arul Arulrajah (2019) Palm oil fuel ash-soft soil geopolymer for
subgrade applications: strength and microstructural evaluation, Road Materials and Pavement
Design, 20:1, 110-131, DOI: 10.1080/14680629.2017.1375967

To link to this article: https://doi.org/10.1080/14680629.2017.1375967

Published online: 14 Sep 2017.

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Road Materials and Pavement Design, 2019
Vol. 20, No. 1, 110–131, https://doi.org/10.1080/14680629.2017.1375967

Palm oil fuel ash-soft soil geopolymer for subgrade applications: strength
and microstructural evaluation
Patimapon Sukmaka , Gampanart Sukmaka , Suksun Horpibulsukb∗ , Monthian Setkita ,
Sippakarn Kassawatc and Arul Arulrajahd
a School of Engineering and Resources, Walailak University, Nakhon Si Thammarat, Thailand; b School
of Civil Engineering, and Center of Excellence in Innovation for Sustainable Infrastructure Develop-
ment, Suranaree University of Technology, Nakhon Ratchasima, Thailand; c Faculty of Commerce and
Management, Prince of Songkla University, Trang Campus, Trang, Thailand; d Department of Civil and
Construction Engineering, Swinburne University of Technology, Melbourne, Australia

(Received 17 February 2017; accepted 22 August 2017 )

This paper presents the strength and microstructural properties of a geopolymer stabilised
soft soil (SS) using palm oil fuel ash (POFA) as a precursor. The liquid alkaline activator,
L used was a mixture of sodium silicate solution (Na2 SiO3 ) and sodium hydroxide solution
(NaOH). Compressive strengths were measured to assess the viability of POFA-SS geopoly-
mer as a stabilised subgrade. Specialised tests were undertaken on POFA-SS geopolymers to
investigate the geopolymerisation mechanisms under various Na2 SiO3 :NaOH ratio, L con-
tent and POFA:SS ratio. These specialised tests included; X-ray diffraction, scanning electron
microscope with energy dispersive X-ray spectroscopy (SEM/EDX) and Fourier transform
infrared (FTIR) spectroscopy tests. The lower POFA:SS ratios required more NaOH and L to
be absorbed by both external and internal negative layer surfaces of SS to develop the sta-
bilised soil structure. The optimum Na2 SiO3 :NaOH ratios providing the highest strength were
at 40:60, 50:50, and 60:40 for POFA:SS ratios of 30:70, 40:60, and 50:50, respectively. The L
providing the highest strength was determined at the optimum liquid alkaline activator content,
OLC (L = 22.8%), 1.2OLC (L = 31.4%) and 1.4OLC (L = 44.55%) for POFA:SS ratios at
30:70, 40:60, and 50:50, respectively. The main chemical products in POFA-SS geopolymers
were calcium aluminate silicate hydrate (C–A–S–H) and calcium sodium aluminate silicate
hydrate (C–(N)–A–S–H).
Keywords: geopolymer; strength; microstructure; soft soil; palm oil fuel ash

1. Introduction
The majority of the population in the southern region of Thailand live in coastal areas where the
ground improvement works is often required prior to the construction of commercial and public
infrastructures. Nakhon Si Thammarat, a large city in the southern region, is underlain by soft
compressible clay and peaty soil deposits. The chemical stabilisation of soft soil (SS) deposits
is commonly undertaken prior to the construction of road embankments and highways in this
congested lowland area.
Currently the soil-cement mixing technique by jet grouting to create a stabilised composite
soil is widely adopted for soft clay stabilisation (Horpibulsuk, Miura, Koga, & Nagaraj 2004;
Horpibulsk, Rachan, Suddeepong, & Chinkulkijniwat, 2011; Horpibulsuk, Chinkulkijniwat,

*Corresponding author. Email: suksun@g.sut.ac.th

© 2017 Informa UK Limited, trading as Taylor & Francis Group

 Road Materials and Pavement Design 111

Cholphatsorn, Suebsuk, & Liu, 2012; Shen, Wang, Horpibulsuk, & Kim, 2013; Shen, Wang,
Sun, Wang, & Horpibulsuk, 2013; Tan, Goh, & Yong, 2002). Portland cement is widely used for
soil stabilisation (Barbosa, MacKenzie, & Thaumaturgo, 2000; Chinkulkijniwat & Horpibulsuk,
2012; Horpibulsuk, Katkan, Sirilerdwattana, & Rachan, 2006), however its production consumes
significant energy coupled with high CO2 emissions. The production of 1 ton of cement can gen-
erate approximately 1 ton of CO2 (Khedari, Watsanasathaporn, & Hirunlabh, 2005). As a result,
the use of alternative low carbon binders to Portland cement for soil stabilisation projects has
generated significant interest world-wide.
Alkali activated geopolymer binders are still at the early stages of development (Pacheco-
Torgal, Abdollahnejad, Camões, Jamshidi, & Ding, 2012) and can potentially produce better
mechanical properties than Portland cement (Salih, Ali, & Farzadnia, 2014). Alkali activated
materials are produced through the reaction of an alumino-silicate normally supplied in powder
form as an industrial by-product or other inexpensive materials (pozzolanic material) with an
alkaline activator, which is usually a concentrated aqueous solution of alkali hydroxide, sil-
icate, carbonate, or sulphate (Provis, 2014). The engineering properties of geopolymers that
are sought for civil engineering applications include: high compressive strength (Amnadnua,
Tangchirapat, & Jaturapitakkul, 2013; Bagheri & Nazari, 2014; Duxson, Provis, Lukey, & van
Deventer, 2007), rapid controllable setting and hardening (Lee & Van Deventer, 2002), fire
resistance (Cheng & Chiu, 2003; Sakkas, Panias, Nomikos, & Sofianos, 2014; Sarker, Kelly,
& Yao, 2014), various acids and salt solution resistance (Palomo et al., 1999; Sukmak, De
Silva, Horpibulsuk, & Chindaprasirt, 2015), high durability against wetting and drying cycles
(Arulrajah et al., 2015; Hoy, Rachan, Horpibulsuk, Arulrajah, & Mirzababaei, 2017); lack of
deleterious alkali–aggregate reactions and low shrinkage (Zhang, Guo, El-Korchi, Zhang, & Tao,
2013).
Alumino-silicate materials, such as kaolin, fly ash (FA), bottom ash, rice husk ash, and palm
oil fuel ash (POFA) (Chindaprasirt & Rukzon, 2008; Salih et al., 2014; Sukmak, Horpibul-
suk, & Shen, 2013; Horpibulsuk, Suksiripattanapong, Samingthong, Rachan, & Arulrajah, 2015;
Tangchirapat, Saeting, Jaturapitakkul, Kiattikomol, & Siripanichgorn, 2007) can be used as a
precursor to react with the liquid alkaline activator. POFA is produced by burning the fibre,
shells and empty fruit bunches of palm oil trees at 800–1000°C to create a fuel to heat steam for
electricity generation purposes (Chindaprasirt, Homwuttiwong, & Jaturapitakkul, 2007). POFA
is mainly disposed to landfills, which causes negative environmental impacts such as pollution of
the air, land, and water as well as other health related problems. In Thailand, more than 100,000
tons of POFA are generated each year (Chindaprasirt et al., 2007; Tangchirapat et al., 2007).
Recently, POFA has been mixed with other alumino-silicate materials, such as ground granu-
lated blast furnace slag, rice husk ash, and FA, to generate geopolymer concretes (Ariffin, Bhutta,
Hussin, Tahir, & Aziah, 2013; Islam, Alengaram, Jumaat, & Bashar, 2014; Karim, Zain, Jamil,
& Lai, 2013). Sodium silicate (Na2 SiO3 ) and sodium hydroxide (NaOH) are widely used as
alkali activators (Salih et al., 2014). Yusuf, Johari, Ahmad, and Maslehuddin (2014a) and Yusuf,
Johari, Ahmad, and Maslehuddin (2014b) evaluated the compressive strength and microstruc-
ture of geopolymer binders developed from a combination of ultra-fine POFA and ground blast
furnace slag cured at a low temperature (60°C). POFA and FA blends were used as precursor
and oil palm shell were used as aggregates to produce lightweight foamed geopolymer concrete
without Portland cement (Liu, Alengaram, Santhanam, Jumaat, & Mo, 2016). POFA and FA
geopolymer concrete would result in similar compressive strength (25 MPa) to ordinary Portland
cement concrete after 28 days (Khankhaje et al., 2016). The study indicated that the geopolymer
binder with the mix of low content of ultra-fine POFA and ground blast furnace slag cured at
60°C resulted in very high compressive strengths.
112 P. Sukmak et al.

For geotechnical and pavement applications, FA, calcium carbide residue and ground
granulated blast furnace slag (Arulrajah et al., 2015; Phetchuay, Horpibulsuk, Arulrajah,
Suksiripattanapong, & Udomchai, 2016; Phummiphan et al., 2016; Phummiphan, Horpibulsuk,
Phoo-ngernkham, Arulrajah, & Shen, 2017; Sukmak, Horpibulsuk, & Shen, 2013; Sukmak,
Horpibulsuk, Shen, Chindaprasirt, & Suksiripattanapong, 2013; Suksiripattanapong, Horpibul-
suk, Chanprasert, Sukmak, & Arulrajah, 2015; Yu, Du, Jin, & Liu, 2016) have been used
as precursors for geopolymers in soil stabilisation. However, the research and application of
silica-rich POFA as a precursor for the geopolymerisation of soft clay at an ambient room tem-
perature is very limited, thus is the focus of this research. The POFA has a low aluminium but
high calcium content. The POFA-SS geopolymer can be applied as a subgrade material in the
southern region of Thailand, where both POFA and SS are abundantly found. The optimum
Na2 SiO3 :NaOH ratio, liquid alkaline activator (L) content and POFA:SS ratio for POFA-SS
geopolymer in subgrade applications were investigated in this research. The effects of curing
time on the strength development in POFA-SS geopolymer were also investigated under an ambi-
ent temperature (27–30°C). The effects of Na2 SiO3 :NaOH ratio, L content, POFA:SS ratios on
the growth of the geopolymerisation products were examined using a scanning electron micro-
scope with energy dispersive X-ray spectroscopy (SEM/EDX), X-ray diffraction (XRD), and
Fourier transform infrared (FTIR) spectroscopy. The knowledge gained from this research can
be extended to other stabilised pavement applications using POFA as a precursor. This research
will be useful for countries that cultivate palm oil in Asia, Latin America, and West Africa,
including Malaysia, Indonesia, Brazil, etc. The outcome of this study leads to the use of POFA
waste products in sustainable SS stabilisation for subgrade application.

2. Materials and methods

2.1. SS, POFA, and liquid alkaline activator
SS samples were collected from the Pak Phanang estuary, Nakhon Si Thammarat province in the
southern part of Thailand, at a depth of 3–4 m. Table 1 shows the properties of SS, indicating
that the specific gravity was 2.62, and the liquid and plastic limits were approximately 59.5%
and 30.7%, respectively. The sample consists of 25% silt and 75% clay (Figure 1). The natural
water content was 36.0%. According to the Unified Soil Classification System (USCS), the SS
was classified as high plasticity (CH). Table 2 and Figure 2 shows the chemical and mineralog-
ical compositions of the soil sample obtained by X-ray fluorescence (XRF) and XRD analysis,
respectively. The loss of ignition (LOI) was determined based on ASTM D 7348 (ASTM, 2007).
Quartz, muscovite and kaolinite were the main mineral components of the SS. Figure 3(a) depicts
the EDX spectrums and the major elements present in the SS, which includes Si, O, C, Fe, and

Table 1. Properties of SS and POFA.

Properties SS POFA

Sand content (%) – 75

Silt content (%) 25 25
Clay content (%) 75 –
Liquid limit (%) 59.5 –
Plastic limit (%) 30.7 –
Water content (%) 36.0 –
USCS classification CH –
Specific gravity 2.62 1.85
 Road Materials and Pavement Design 113

Figure 1. Grain size distribution curves of POFA and SS.

Table 2. Chemical composition of SS and POF.

Composition SS (wt%) POFA (wt%)

SiO2 60.12 56.31

K2 O 2.03 5.7
Fe2 O3 10.04 1.68
CaO 0.93 14.24
P2 O5 N.D 1.67
MgO 0.01 8.61
Al2 O3 13.19 4.7
SO3 0.16 2.55
TiO2 1.7 0.39
Na2 O 0.6 0.16
MnO 0.65 0.41
CuO N.D 0.1
Rb2 O 0.06 0.05
ZnO N.D 0.06
Cr2 O3 0.01 N.D
LOI 10.5 3.37

Al. According to Table 2, the identified elements by EDX test were compatible with the chem-
ical compositions obtained by XRF, in that the SS consisted of a high content of silica and low
contents of magnesium and potassium, and its alumina content is 13.19%. As shown in Figure 4,
the compaction characteristics under modified Proctor energy (ASTM D1557) were an optimum
water content (OWC) of 22% and a maximum dry unit weight, γ d,max of 18.9 kN/m3 .
POFA was collected from a mill located in the southern part of Thailand. The temperature of
approximately 800–1000°C was used to burn the palm oil fibres, shells, and empty fruit bunches.
The POFA was oven-dried at 110 ± 5°C for 24 h and sieved through a 1.18 mm sieve in order
to remove foreign materials and larger particles. The specific gravity of POFA was 1.85. Table 1
depicts the chemical and mineralogical compositions of POFA obtained by XRF, where the major
components evidently contained mainly SiO2 and CaO at 56.31% and 14.24%, respectively,
with a small amount of Al2 O3 (4.7%). The POFA had a SiO2 + Al2 O3 + Fe2 O3 of 62.69%,
SO3 = 2.55%, and LOI = 3.37%. According to ASTM C 618, it can be classified as a Class C
FA (SiO2 + Al2 O3 + Fe2 O3 > 50%, SO3 < 5%, and LOI < 6%). Figure 2 describes the XRD
patterns for POFA, indicating major phases of alpha quartz, cristobalite, and calcite (Chandara,
114 P. Sukmak et al.

Figure 2. XRD of (a) POFA and (b) SS.

Figure 3. SEM/EDX photos of (a) SS and (b) POFA.

 Road Materials and Pavement Design 115

Figure 4. Relationships between total unit weight and water content of the compacted POFA-SS blends
at various POFA:SS ratios.

Sakai, Azizli, Ahmad, & Hashim, 2010; Kroehong, Sinsiri, Jaturapitakkul, & Chindaprasirt,
2011). Figures 1 and 3 depict the grain size distribution curves and SEM/EDX of POFA after
sieving as compared with those of the SS. The grain size distribution of SS was found to be finer
than that of POFA. The mean particle size (d50 ) of POFA was 107 μm, which was larger than that
of SS (d50 = 1.04 μm). The morphology of POFA consisted of irregular shaped particles with
porous cellular surfaces, similar to that of the SS particles. Figure 3(b) shows the EDX spectrums
of POFA, indicating that major elements present were O, Si, C, Ca, K, and Mg, compatible with
the chemical compositions of POFA obtained by XRF.
The liquid alkaline activator, L used to induce geopolymerisation of the SS was a NaOH and
Na2 SiO3 solution. Commercially available reagent grade NaOH had 98% purity and Na2 SiO3
was composed of 9% Na2 O, 30% SiO2 , and 61% water.

2.2. Specimen preparation of POFA-SS blends

The POFA-SS blend was a mixture of POFA, SS, and water. The POFA:SS ratios studied were
at 30:70, 40:60, and 50:50. The POFA-SS blends were prepared at different water contents under
modified Proctor compaction energy (ASTM D 1557) in order to investigate their initial strength
without liquid alkaline activators. Based on the predetermined Proctor compaction curves, the
blends at various POFA:SS ratios were statically compressed at the corresponding OWC in a
cylindrical mould, 50 mm in diameter and 100 mm in height, with a manual hydraulic jack to
attain the γ d,max . By this procedure, all specimens had the same compression (modified Proctor)
energy per volume. The OWC value at any compaction energy can be rapidly approximated using
the one point test (Blotz, Benson, & Boutwell, 1998; Horpibulsuk, Katkan, & Apichatvullop,
2008; Horpibulsuk, Katkan, & Naramitkornburee, 2009). The specimens were then dismantled
and immediately wrapped within a vinyl sheet to minimise the water evaporation during curing
at ambient temperature (27–30°C).

2.3. Specimen preparation of POFA-SS geopolymer

The POFA-SS geopolymer was a mixture of SS at natural water content, POFA, and L. The
POFA:SS ratios were at 30:70, 40:60, and 50:50. The L was prepared by varying Na2 SiO3 :NaOH
116 P. Sukmak et al.

ratios at 0:100, 20:80, 40:60, 50:50, 60:40, 80:20, and 100:0. The concentration of NaOH was
fixed at 10 molars. The POFA and SS were thoroughly mixed with L and then compacted under
modified Proctor energy according to ASTM D1557. The optimum liquid alkaline activator
content (OLC) of specimens at different ratios of Na2 SiO3 :NaOH and POFA:SS was then deter-
mined. The POFA-SS geopolymers at an L between 0.8OLC and 1.8OLC were prepared based
on the same compression and curing procedure as the POFA-SS blends.

2.4. Unconfined compressive strength test

The unconfined compressive strength (UCS) values of the POFA-SS blends and POFA-SS
geopolymers were measured after 7, 14, 28, 60, and 90 days of curing according to ASTM D
1633. In order to obtain reliable test results, the reported results were the average of at least five
specimens. Under the same testing conditions, most cases were reproducible with a low standard
deviation, SD (SD/x̄ < 10%, where x̄ is the mean strength value).
According to the Department of Highways (DOH) and the Department of Rural Roads, Thai-
land as well as road authorities in Australia and other countries, the UCS is the critical design
parameter and as such was used for comparison purposes in this study. Cyclic tests such as
resilient modulus and permanent strain, typically used for the mechanistic design procedure, are
recommended for future studies.

2.5. Microstructural test

In this study, XRD, FTIR spectra, and SEM/EDX were used to examine the growth of the
geopolymerisation structure on the specimens. XRD was used to determine the phases present
in the specimens and FTIR to identify different types of chemical bonds present in the materials
at a molecular level. A XRD analysis was done using the Bruker D2 Phaser from 5 to 80 of
2θ°. The diffraction patterns were analysed using Expert High Score Plus software. For FTIR,
the equipment used was FTIR Spectrometer Tensor 27 (Bruker). Approximately 5 mg of pow-
dered specimens was mixed with 95 mg of potassium bromide (KBr). The powder was pressed
for 2 min under 2.758 MPa by hydraulic pressing to prepare the translucent pellets, which were
then inserted into the infrared spectrometer. The infrared spectra were recorded in the range of
550–5000 cm−1 wavelength. The SEM/EDX specimens were broken from the centre into small
fragments. Subsequently, the specimens were frozen at − 195°C by immersion in liquid nitrogen
for 5 min and evacuated at a pressure of 0.5 Pa at − 40°C for 5 days to remove moisture from the
solid state (Sukmak, Horpibulsuk, Shen, et al., 2013). Prior to SEM/EDX analysis, all specimens
were coated with gold. The SEM and EDX were performed using Merlin compact, Zeiss and
Oxford, Aztec, respectively.

3. Results
Figure 4 shows the relationships between total unit weight and water content of the POFA-SS
blends at various POFA:SS ratios. It is apparent from Figure 4 that the maximum total unit weight
of POFA-SS blends at all POFA:SS ratios are lower than that of SS. Higher POFA:SS ratios
result in lower maximum total unit weights. Generally, gradation and specific gravity control the
compaction curve (Sukmak, Horpibulsuk, Shen, et al., 2013). The POFA has a lower specific
gravity than that of SS, hence the POFA-SS blends possess a lower total unit weight.
Figure 5 shows the plots of total unit weight versus L of POFA-SS geopolymers at var-
ious POFA:SS and Na2 SiO3 :NaOH ratios. It is apparent from Figure 5, that for a given
POFA:SS ratio, the compaction curves of POFA-SS geopolymers are approximately similar for
 Road Materials and Pavement Design 117

Figure 5. Plots of total unit weight versus L content of compacted POFA-SS geopolymer at various ratios
of POFA:SS and Na2 SiO3 :NaOH ratios, under modified Proctor energy.

Figure 6. Effects of water content and POFA:SS ratio ratio on strength development for POFA-SS blends.

all Na2 SiO3 :NaOH ratios. The decrease in maximum total unit weight is associated with the
increase in OLC (Sukmak, Horpibulsuk, Shen, et al., 2013). It is evident from Figures 4 and 5
that the POFA-SS geopolymers have higher total unit weights than the POFA-SS blends at all the
POFA:SS ratios. This can be possibly attributed to soil flocculation during the geopolymerisation
reaction.
Figure 6 shows the effects of water content and POFA:SS ratios on UCS development in
the POFA-SS blends after 28 days of curing. For a given POFA:SS ratio, the UCS of POFA-
SS blend increases with water content up to the OWC (densest package) and decreases when the
water content is on the wet side of OWC, which is typical of compacted clay behaviour (Sukmak,
Horpibulsuk, Shen, et al., 2013). The UCS decreases with increasing POFA:SS ratio because the
increase in POFA reduces the soil cohesion of the blends (Figure 4).
Figure 7 shows the effect of L and POFA:SS ratio on strength development in POFA-
SS geopolymers. Similar to the POFA-SS blend, the UCS of POFA-SS geopolymer at
118 P. Sukmak et al.

Figure 7. Effects of L and POFA:SS ratio on strength development for POFA-SS geopolymers.

POFA:SS = 30:70 increases with L up to the OLC (densest package) and decreases when L
is on the wet side of OLC. When L is much lower than the OLC, the strength is insignificant
since the amount of L is insufficient to leach the silicon and aluminium in the amorphous phase
of POFA for the geopolymerisation process. The UCS reduction at very high L (L more than
OLC) is because the amount of OH− from the liquid alkaline activator causes precipitation at
the very early stages before the poly-condensation process of geopolymerisation (Sukmak, Hor-
pibulsuk, & Shen, 2013). Unlike POFA:SS = 30:70, the maximum UCS for higher POFA:SS
ratio is found at L > OLC. For POFA:SS = 40:60 and 50:50, the maximum UCS is found
at L = 1.2OLC (L = 31.4%) and L = 1.4OLC (L = 44.55%), respectively. This implies that
for POFA:SS = 40:60 and 50:50, the L = OLC is just sufficient for compression, but not for
geopolymerisation. It is evident that the maximum 7-day UCS values of POFA-SS geopolmers
at POFA:SS = 30:70, 40:60, and 50:50 meet the strength requirement (UCS > 294.2 kPa) for
stabilised subgrade specified by the DOH (DH-S102/2532).
 Road Materials and Pavement Design 119

Figure 8. Relationship between compressive strength and curing time of POFA-SS blend and POFA-SS
geopolymer for various Na2 SiO3 :NaOH ratios and curing times at 7, 14, 28, 60, and 90 days.

Figure 8 shows the UCS development over curing time of POFA-SS blends at OWC and
POFA-SS geopolymers at OLC for various Na2 SiO3 :NaOH ratios. The UCS development in
POFA-SS geopolymers is controlled by three influence factors; namely Na2 SiO3 :NaOH ratio,
POFA:SS ratio and the curing time. The optimum Na2 SiO3 :NaOH ratios providing the high-
est UCS are found at 40:60, 50:50, and 60:40 for POFA:SS ratios of 30:70, 40:60, and 50:50,
respectively. Since the SS contains alumino-silicates layers with both external and internal neg-
ative layer surfaces, the lower POFA:SS (higher SS content) requires a higher NaOH and L.
The negative layers act as a huge anion and a swarm of positively charged cations such as Na+ ,
K+ , Ca2+ , and Mg2+ (Soga & Mitchell, 2005; Sukmak, Horpibulsuk, & Shen, 2013). Therefore,
some of the input NaOH content to leach the silicon and aluminium in the amorphous phase of
POFA were absorbed by the negative charges between negative layers to form an ionic inter-
layer. As a result, the POFA:SS ratio at 30:70 needs more NaOH and L for geopolymerisation
120 P. Sukmak et al.

Figure 9. XRD diffractogram of (a) POFA-SS geopolymer at 0.8OLC, (b) POFA-SS geopolymer at OLC,
and (c) POFA-SS geopolymer at 1.2OLC for POFA:SS = 30:70.

than the POFA:SS ratios at 40:60 and 50:50. The UCS values of POFA-SS geopolymers for all
POFA:SS ratios increases rapidly in the first 28 days of curing. After 60 days, the UCS devel-
opment is insignificant. The same is however not true for POFA-SS blends, whereby the UCS
development with time for all POFA:SS ratios is insignificant. It is indicative that the UCS devel-
opment strongly depends on the reaction between the POFA and the liquid alkaline activator for
generating geopolymerisation reaction (Phoo-ngernkham, Chindaprasirt, Sata, Hanjitsuwan, &
Hatanaka, 2014; Sukmak, Horpibulsuk, Shen, et al., 2013).

4. Microstructural analysis
The role of L on the UCS development in POFA-SS geooplymer is shown in Figure 9, which
compared the XRD patterns of POFA-SS geopolymers at POFA:SS = 30:70 after 28 days at
various L. Figure 9(a)—(c) shows the XRD patterns of the POFA-SS geopolymer specimens at
different L values ranging from (0.8–1.2) OLC. The peak intensities of quartz, muscovite, and
kaolinite of crystalline components from the POFA and SS are clearly evident. The calcite peaks
are moreover significantly detected with the appearance of calcium aluminate silicate hydrate
peak (gismondine, C–A–S–H) at about 20.80 and 27.97°2θ and calcium sodium aluminium sil-
icate hydrate peak (gismondine, C–(N)–A–S–H) at about 20.94 and 30.07°2θ . The geopolymer
specimen at OLC shows the highest intensity of gismondine peak compared to the specimens at
0.8OLC and 1.2OLC. As such, the maximum UCS value is found at OLC.
SEM images for the POFA-SS blends and POFA-SS geopolymers at POFA:SS = 30:70 are
shown in Figure 10. The POFA-SS blend at OWC (Figure 10(a)) exhibits the flocculated struc-
ture with very dense packing. As such, the compacted specimen at OWC possesses the highest
 Road Materials and Pavement Design 121

UCS as shown earlier in Figure 6. Unlike the POFA-SS blend, the UCS of the POFA-SS geopoly-
mers is enhanced by both the mechanical and chemical components. The mechanical component
is primarily governed by soil densification, whereas the OLC provides the densest packing
(Figure 7(a)). At a low L content (0.8OLC) (Figure 10(b)), geopolymerisation products are less
present, since some L is taken by the SS particles for developing the soil structure. The low alka-
line activated condition (low amount of OH− ) is therefore insufficient to leach the silicon and
aluminium for generating geopolymerisation products. By increasing the L content, the POFA
and SS particles come closer due to the solution lubrication and more geopolymerisation reaction
(Figure 10(c)). Hence, the strength of the POFA-SS geopolymers increases with L content up to
the highest value at the OLC (Figure 7) for POFA:SS ratio of 30:70. Beyond this L content, the
micro-cracks on the POFA particles were found (Figure 10(d)) due to the precipitation at the
very early stages prior to the poly-condensation process of geopolymerisation in the excessive
alkaline activated condition.
Figure 11 shows the SEM images of the POFA-SS geopolymers for POFA:SS = 40:60 and
50:50 at various L. Figure 11(a) shows the SEM image for POFA:SS = 40:60 at OLC while
Figure 11(b) and 11(c) shows the SEM images for POFA:SS = 40:60 on the wet side of OLC.
Figure 11(d) shows the SEM image for POFA:SS = 50:50 at OLC while Figure 11(e) and 11(f)
shows the SEM images POFA:SS = 50:50 on the wet side of OLC. Figure 11(a) and 11(d) (at
OLC for POFA:SS = 40:60 and 50:50) shows that the alkaline activated condition is insufficient
to leach the silicon and aluminium for producing alumina-silicate gel resulting in less geopoly-
merisation products. At 1.4OLC and 1.6OLC for POFA:SS of 40:60 and 50:50, respectively,
the excessive L causes micro-cracks on POFA particle with less alumina-silicate gel, hence the
resulting strength reduction. Figure 11(b) and 11(e) shows the highest amount of geopolymerisa-
tion products on the POFA particles, SS particles and in the pores (Jiminez, Lachowski, Palomo,
& Macphee, 2004). Consequently, at these L value, the specimens possess the highest strength
(Figure 8).
To trace the geopolymerisation products, EDX was conducted on specimens with
POFA:SS = 30:70. Three points with different morphologies were selected and examined and
are presented in Figure 10. The major elements present include O, Si, Na, Ca, C, K, Al, P, and
Mg. The elements identified by the EDX test are compatible with the chemical composition of
the POFA and SS (Table 1). A low content of alumina and a high content of silica and calcium
are found in the POFA, while a low content of calcium and a high content of silica and alumina
are found in the SS. The high contents of Si, Na, and Ca and a low content of Al in the EDX
spectroscopy results indicate that the geopolymer products are mostly a result of formation of
C–A–S–H and C–(N)–A–S–H as reported in the XRD pattern (Figure 9).
Figure 12 presents the FTIR results for the POFA (Figure 12(a)), SS (Figure 12(b)), and POFA-
SS geopolymers at a POFA:SS ratio of 30:70 (Figure 12(c)). POFA exhibits a broad band around
∼ 1010 cm−1 , which is associated with the stretching vibration mode of Si–O–Si bonds of SiO2
(Mijarsh, Johari, & Ahmad, 2014). Also, bands at 693 and 713 cm−1 associated with the asym-
metric vibration mode of the quartz double band (Criado, Palomo, & Fernández-Jiménez, 2005),
at 795 cm−1 attributed to the bending vibration mode of the Si–O–Si bonds (Bakharev, 2005),
at 875 cm−1 associated with the asymmetric vibration mode of the Al–O–H (Yunsheng, Wei, &
Zongjin, 2007), at ∼ 1440 cm−1 associated with the asymmetric vibration mode of the O–C–O
bonds in carbonates, at 1650 cm−1 attributed to the stretching vibration mode of the (–OH, HOH)
(Ylmén, Jäglid, Steenari, & Panas, 2009) and at ∼ 2984 cm−1 associated with the vibration mode
of the calcium carbonates band (Ylmén et al., 2009) are detected. The FTIR spectrum of SS is
different from that of POFA. The band at 1440 cm−1 disappears while the band at the 690 cm−1
region attributed to the vibration mode of the Al–O (Pansu & Gautheyrou, 2007) is detected.
The band around ∼ 1010 cm−1 for POFA is lower than that at 1015 cm−1 for SS that is similarly
122 P. Sukmak et al.

associated with the stretching vibration mode of the Si–O–Si bonds of silicon dioxide tetrahedral
due to a high silica in SS (Bernal, Rodríguez, de Gutiérrez, Provis, & Delvasto, 2012). More-
over, the band at 693 and 713 cm−1 for POFA is lower than that of SS at 779 and 796 cm−1 that
is associated with the asymmetric vibration mode of the quartz double band (Criado et al., 2005).

Figure 10. SEM/EDX images of (a) POFA-SS blend at OWC, (b) POFA-SS geopolymer at 0.8OLC, (c)
POFA-SS geopolymer at OLC, and (d) POFA-SS geopolymer at 1.2OLC for POFA:SS = 30:70.
 Road Materials and Pavement Design 123

Figure 10. Continued.

A new vibration band is also indicated at the 938 cm−1 that is associated with the deformation
external of –OH bonds (Pansu & Gautheyrou, 2007).
In this study, the differences between the FTIR absorption frequencies for the POFA, SS, and
POFA-SS geopolymers show evidence of geopolymerisation. Bands indicated for POFA at 875
and 2984 cm−1 disappear and the main characteristic bands of the vibration spectra signalled at
regions of 1010–1015 cm−1 for POFA and SS are shifted to lower frequencies at wave num-
ber region 982 cm−1 , indicating stretching vibration of Si–O–Al or Si–O–Si chains. This can be
correlated to the increase in the number of Si–O–(Si,Al) bonds (C–A–S–H and C–(N)–A–S–H)
124 P. Sukmak et al.

due to more cross linked (N–A–S–H) and (C–S–H) binder gels, resulting in the UCS improve-
ment. The observation from both XRD and FTIR is well correlated and explains the formation
of the gel binder (C–A–S–H and C–(N)–A–S–H) in the POFA-SS geopolymers. The products

Figure 11. SEM images of POFA- SS geopolymer for (a) POFA:SS = 40:60 at OLC, (b)
POFA:SS = 40:60 at 1.2OLC, (c) POFA:SS = 40:60 at 1.4OLC, (d) POFA:SS = 50:50 at OLC, (e)
POFA:SS = 50:50 at 1.4OLC, and (f) POFA:SS = 50:50 at 1.6OLC.
 Road Materials and Pavement Design 125

Figure 11. Continued

126 P. Sukmak et al.

Figure 11. Continued

of the reaction between calcium precusors and alkali metal silicates or hydroxide solutions are
generally dominated by an aluminium substituted calcium silicate hydrate gel (C–A–S–H and
C–(N)–A–S–H), which is tobermorite and is broadly comparable to the gel structure resulting
from Portland cement hydration. Substitution of Al in the CSH structure led to a higher degree of
polymerisation and degree of crosslinking between tobermorite chains. Furthermore the available
 Road Materials and Pavement Design 127

Figure 12. FTIR results for (a) POFA, (b) SS, and (c) POFA-SS geopolymer at POFA:SS = 30:70.

Na from the alkali activators absorbed onto the gel itself and can be written as C–(N)–A–S–H
(gismondine) (Provis, 2014).
The present study on the improvement of SS by POFA based geopolymer has significant
impacts on sustainable pavement applications. The field construction will begin with roller-
compaction of the underlying subgrade in accordance with the specifications of the road
authority. The SS will be mixed with POFA at the construction site or in a ready mixer from
a plant. A mixture of SS and POFA will be activated by the liquid alkali activator at the opti-
mum content. Subsequently, the SS-POFA geopolymer will be compacted to attain a minimum
modified Proctor density of 95%.

5. Conclusions
In this study, POFA was used as a precursor in POFA-SS geopolymers. To assess the applicability
of POFA as a single source of alumino-silicate in geopolymerisation, extensive mechan-
ical and microstructural tests were performed. The influence factors investigated included
Na2 SiO3 :NaOH ratio, L content, POFA:SS ratio, and curing time. The following conclusions
can be drawn from this research:

(1) The maximum total unit weight of both compacted POFA-SS blends and compacted
POFA-SS geopolymers at the various POFA:SS ratios was lower than that of compacted
128 P. Sukmak et al.

SS. The higher POFA:SS ratio results in a lower maximum total unit weight because the
specific gravity of POFA was lower than that of SS. Due to soil flocculation during the
geopolymerisation reaction, the total unit weights of the compacted POFA-SS geopoly-
mers were higher than those of the compacted POFA-SS blends at the same POFA:SS
ratios.
(2) The higher SS, containing alumino-silicates layers with both external and internal
negative layer surfaces, required more NaOH and L content for the geopolymerisa-
tion reaction to occur. Consequently, the optimum Na2 SiO3 :NaOH ratio and L content
providing the highest strength were at 40:60 and OLC (22.8%), 50:50 and 1.2OLC
(L = 31.4%), and 60:40 and 1.4OLC (L = 44.55%) for POFA:SS = 30:70, 40:60, and
50:50, respectively.
(3) The microstructural analysis showed that the L contents on the dry side of optimum L
were insufficient to leach the silicon and aluminium for generating geopolymer products,
while the L contents on the wet side of optimum L caused precipitation at the very early
stages before the poly-condensation process in the geopolymers, as evident from the
micro-cracks on the POFA.
(4) The samples with maximum UCS showed the highest cementitious products. The main
cementitious products detected were gismondine (C–A–S–H and C–(N)–A–S–H).
(5) The 7-day UCS values of the POFA-SS geopolymers at OLC, 1.2OLC and 1.4OLC
for POFA:SS = 30:70, 40:60, and 50:50, respectively, were found to meet the strength
requirement of subgrade materials specified by the DOH, Thailand.

Disclosure statement
No potential conflict of interest was reported by the authors.

Funding
This work was supported by Walailak University: [grant number WU60102]; Suranaree University of
Technology; Thailand Research Fund [grant number RTA5980005].

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