Construction and Building Materials 93 (2015) 2934

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Construction and Building Materials

journal homepage: www.elsevier.com/locate/conbuildmat

The effects of high volume nano palm oil fuel ash on microstructure
properties and hydration temperature of mortar
Nor Hasanah Abdul Shukor Lim a, Mohamed A. Ismail b,, Han Seung Lee b, Mohd Warid Hussin c,
Abdul Rahman Mohd. Sam c, Mostafa Samadi a
a
b
c

Construction Material Research Group (CMRG), Faculty of Civil Engineering, Universiti Teknologi Malaysia, 81310 UTM Johor Bahru, Johor, Malaysia
Dept. of Architectural Engineering, Hanyang University, Ansan, Republic of Korea
Construction Research Centre (UTM CRC), Institute for Smart Infrastructure and Innovative Construction, Universiti Teknologi Malaysia, 81310 UTM Johor Bahru, Johor, Malaysia

h i g h l i g h t s
 High volume of nano POFA as cement replacement improves strength.
 Nano POFA reduces hydration temperature of massive concreting in early age.
 Treatment of POFA increases pozzolanic properties and activity index.

a r t i c l e

i n f o

Article history:
Received 3 February 2015
Received in revised form 12 May 2015
Accepted 15 May 2015

Keywords:
Microstructure
Palm oil fuel ash
Mortar strength
High volume
Hydration temperature

a b s t r a c t
The effect of high volume nano palm oil fuel ash in the mortar was investigated. This study covers basic
properties like the morphology of the composite, the hydration temperature, strength activity index,
thermal conductivity and microstructure properties with regards to the variations in the mix design
process of mortar. The effects of neness of the ash on the strength properties of mortar were also
investigated. To get a better performance in terms of strength development, the ash used has gone
through heat treatment and was ground up to less than 1 lm. The incorporation of more than 80% nano
size palm oil fuel ash as cement replacement has produced a mortar having a compressive strength more
than OPC mortar at a later age. The overall results have revealed that the inclusion of high volume nano
palm oil fuel ash can produce a mortar mix with high strength, good quality and most importantly that is
more sustainable.
2015 Elsevier Ltd. All rights reserved.

1. Introduction
Affordable products with advanced properties are necessary
towards the higher human development and sustainable economic
growth. Therefore, reusing the abundant waste materials has
become necessary especially waste coming from palm oil manufacturing. It is estimated that the total potential palm biomass from
4.69 million hectares of palm oil planted area in Malaysia in 2009
is 77.24 million tonnes per year comprising of 13.0 million tonnes
of Oil Palm Trunks (OPT), 47.7 million tonnes of Oil Palm Fronds
(OPF), 6.7 million tonnes of Empty Fruit Bunches (EFB), 4.0 million
tonnes of Palm Kernal Shell (PKS) and 7.1 million tonnes of
Mesocarp Fibre (MF) (all dry weight) [1,2]. These wastes are usually used as fuel in palm oil mill to generate electricity [3] and after
Corresponding author. Tel.: +82 31 4005181; fax: +82 31 4368169.
E-mail address: mismail@hanyang.ac.kr (M.A. Ismail).
http://dx.doi.org/10.1016/j.conbuildmat.2015.05.107
0950-0618/ 2015 Elsevier Ltd. All rights reserved.

the combustion in the boiler there are approximately 5% of ash

generated [4] and another solid waste being produced. The need
towards sustainability and sustainable environment has made
the use of pozzolanic material in mortar popular. One of the latest
additions of pozzolanic material is palm oil fuel ash (POFA) [57].
This POFA is the source of silicate that produced after the
combustion of palm oil bre, shell and mesocarp as fuel to
generate electricity [8]. Few studies were done by other researchers on the replacement of partial weight of cement by POFA [9,10],
but there is still high amount of ash abundant in the landll which
lead to environmental problems. It is reported that the maximum
strength gain occurred at the replacement level of 30% with the
size of 45 lm but further increment in the ash content would
reduce the strength of mortar gradually [5]. Besides, POFA was also
used as nano ller [11].
The hydration temperature of mortar describes the hardening
behaviour of it. The mix properties and component of materials

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Nor Hasanah Abdul Shukor Lim et al. / Construction and Building Materials 93 (2015) 2934

used in mortar have too much effect on hydration temperature.

The heat released in hydration process of mortar containing
blended ash is originating from two reactions rstly heat released
from hydration of cement and secondly heat released from admixture reactions [12]. Therefore, exploring POFA as nano material
would create an advanced waste material. In this paper, high
volume of POFA with size less than 1 lm was used as cement
replacement up to 80%. This helps to reduce the hydration temperature and carbon dioxide gasses emission from cement production
process.

Table 1
Mix proportions of mortar.
Materials (kg/m3)

Binder

OPC
GPOFA
UPOFA
Fine aggregate
w/b ratio

Mortar mix
OPC mortar

GPOFA mortar

UPOFA mortar

525

1578
0.4

105
420

1578
0.4

105

420
1578
0.4

Activity index AI A=B  100

2. Materials and methods

2.1. Materials
The cement used in this study complies with Portland cement Type I as stated in
the ASTM C 150-12 [13]. Palm oil fuel ash (POFA) was obtained from the burning of
palm oil shell and husk (in equal volume) from a southern part of Malaysia. The collected ashes were dark in colour and the losses on ignitions (LOI) were 20.9% for
ground POFA. The POFA was then dried in the oven for 24 h at 105 5 C and sieved
through a 150 lm size sieve to remove coarser particles. Then the POFA was ground
up until 90% passing 45 lm sieve according to ASTM C618-12 [14] and mention in
this paper as GPOFA for ground POFA. Meanwhile, the POFA was then heated to
500 C for 1 h in a furnace to remove the excessive unburned carbon [15,16]. The
carbon content is an important factor to consider. These particles result in the
increasing of water demand because it is absorbed by carbon particles [15,17].
Then it was subjected to further grinding using ball mill until it reaches the meridian size of less than 1 lm and in this paper refer to UPOFA for ultrane POFA. To
ensure the uniformity and neness of POFA, all the treatment processes were
controlled [16].
In the preparation process for all specimens, the ne aggregates were used in
the saturated dried surface condition. The ne aggregate was sieved through
2.35 mm sieve and retained at 300 lm before storing in the airtight container.
Fig. 1 shows the sieve analysis test on the ne aggregates. The grading curve for ne
aggregates was within the limit line prescribed according to ASTM C33-03[18].
2.2. Testing procedures
All mortar specimens were prepared with sand to binder with the ratio of 3:1,
whereby the sand was prepared into saturated surface dried condition. The mixing
was carried out in a room temperature of approximately 28 2 C [19]. The mix
proportions are given in Table 1 based on weight of materials according to BS EN
998-1:2010 [20]. The test specimens of 70  70  70 mm cubes were prepared.
The specimens were compacted in two-layer with rod tamping as described in
ASTM C109-13 [21]. Additional vibration of about 10 s was applied using the vibrating table. The test specimens were cured in water for 7, 14 and 28 days.
The morphology of UPOFA was investigated by using Field Emission Scanning
Electron Microscopy (FESEM). The surface of the specimens obtained from the compressive strength test was coated with gold prior to their morphological observation. A thermo gravimetric analysis (TGA) was carried out to investigate the
thermal stability of the composites. The powder (about 25 5 mg) was heated at
a heating rate of 20 C/min from 30 to 800 C under nitrogen. Fourier transforms
infrared spectroscopy (FTIR) which is a tool for qualitative and quantitative materials and identication of the composite group and chemical bonding in mortar
specimens.
The activity index for UPOFA and GPOFA were checked for pozzolanic materials.
As prescribed by ASTM C 311-13 [22], activity index is dened as:

3. Results and discussions

3.1. Chemical and physical properties
The chemical and physical properties of OPC, GPOFA and UPOFA
are shown in Tables 2 and 3, respectively. It reveals that the OPC
and POFA have similar characteristics base on the chemical composition. UPOFA sample contains higher percentage of silica content
than GPOFA and OPC. Obviously, the presence of higher silica content inuences the pozzolanic reaction to produce extra calcium
silicate hydroxide gels thus makes the mortar more durable and
denser. The ndings show that the GPOFA used is classied as
Class C pozzolan meanwhile UPOFA as Class F pozzolan [14] which
conform to the observations made by a previous research [23].
Results show that the heat treatment reduced the LOI of POFA
from 20.9% to 1.3% hence removed the unburned elements in the
POFA. The neness of UPOFA is 146% more than OPC used in this
study. The percentage of particle retain on sieve size 45 micron
are 4.5, 4.9 and 0.13 for OPC, GPOFA and UPOFA, respectively.
Thus, the UPOFA have large surface area and signicantly smaller
particle size in comparing with OPC and GPOFA.

Percentage retained (%)

100
90
80
70

fine aggregate

60

lower limit

upper limit

50
40
30
20
10
0
1

10
Sieve size (m)
Fig. 1. Sieve analysis of ne aggregate.

where A = average compressive strength of POFA mortar cube and B = average compressive strength of control mortar cube.
The compressive strength of the mortar cubes was determined using a 3000 kN
compression machine according to ASTM C109-13 standards [21]. The test was performed on mortar cubes at the ages of 7, 14 and 28 days. For hydration temperature
measurement, plywood with the size of 300  300  450 mm cube was used as the
exterior mould. It was packed with 76 mm thick polystyrene acting as the insulator.
Each mortar mix was cast into PVC pipe with the size of 150 mm diameter and
300 mm heights. The same method was used by other researchers [10,23] to determine the hydration temperature. A thermocouple (Type K) was inserted into the
centre of each box and was connected to a data logger system. Recording the
temperature was continued up to 7 days for the whole mortar types. Fig. 2 shows
the equipment used in the test.

Fig. 2. Test equipment for measuring hydration temperature.

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Nor Hasanah Abdul Shukor Lim et al. / Construction and Building Materials 93 (2015) 2934
Table 2
Chemical composition of OPC, GPOFA and UPOFA.
Chemical composition (%)

OPC

GPOFA

UPOFA

SiO2
Al2O3
Fe2O3
CaO
K2O
MgO
CO2
SO3
LOI

16.40
4.24
3.53
68.30
0.22
2.39
0.10
4.39
2.4

53.5
1.9
1.1
8.3
6.5
4.1
0.30
2.36
20.9

69.3
5.30
5.10
9.15
11.10
4.10
0.10
1.59
1.3

(a) before treatment (GPOFA)

(b) after treatment (UPOFA)

Fig. 4. POFA colour before and after treatment.

Table 3
Physical properties of OPC, GPOFA and UPOFA.
Physical properties

OPC

GPOFA

UPOFA

5.4

Specic gravity
Particle retained on 45 lm sieve
Median particle d10
Median particle d50
Blaine neness (cm3/g)

3.15
4.58

3999

2.42
4.98
1.69
14.58
4935

2.56
0.13
0.02
1.10
7205

5.3

Weight (mg)

3.2. Morphological structure of POFA

5.1
5
4.9
4.8

The morphological structure of UPOFA sample was examined

using Field Emission Scanning Electron Microscope (FESEM) technique. UPOFA consists of thinner, irregular and crushed particles
as a typical microstructure of the ash being shown in Fig. 3. It
can be observed that POFA has irregular, thinner and crushed particle having clustered arrangement of the spherical particles with
little air space between them [9,10].
3.3. Thermogravimetric analysis
The colour of POFA changed from dark black to greyish brown
after the carbon particles were removed as shown in Fig. 4 and this
is similar to the ndings observed by Altwair et al. [24]. Fig. 5
shows the TGA result for the POFA used. The weight loss in the
temperature of 100 5 C was caused by the evaporation of moisture content. The decarbonation of POFA occurs between temperatures of 400 and 600 C. This may be due to the calcium carbonate
decomposition. From the gure, 0.3578 mg of CO2 evaporated during the process as shown below:

CaCO3 s ! CaO s CO2 g

Content 6.8391%
0.3578 mg

5.2

4.7
4.6
0

100

200

300

400

500

600

700

800

900

1000

Temperature (C)
Fig. 5. TGA results for POFA.

Since the suitable temperature for heat treatment is between

400 and 600 C, in this study, POFA was heated up to 500 C for
the duration of only 1 h [14,15].

3.4. Fourier transforms infrared spectroscopy (FTIR) results

Fig. 6 shows the FTIR result of UPOFA and GPOFA. As shown in
the gure, there is large difference between the treated and
untreated POFA. The water component of OH stretching band at
3465 cm1 and the bending of the chemically bonded water, H
OH at 1650 cm1 were altered by the exposure to the treatment
process. The SiO asymmetric stretching vibration mode at
1040 cm1 also showed high shift after treatment. This suggested
that the treatment process alters the chemical structures and

Si-O
GPOFA
UPOFA

H-O-H

O-H

3900

3400

2900

2400

1900

1400

Wavenumbers (cm-1)
Fig. 3. Field Emission Scanning Electron Micrograph of POFA.
Fig. 6. FTIR spectra of UPOFA and GPOFA.

900

400

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Nor Hasanah Abdul Shukor Lim et al. / Construction and Building Materials 93 (2015) 2934

Table 4
Strength activity index results.

50

GPOFA

UPOFA

7 days
28 days

75
84

97
105

increases the chemical composition of the materials. The value of

silica content increased from 0.7 to 3.4 absorbance.

OPC

45

POFA(N)

Temperature (C)

Activity index (%)

POFA(B)
40

35

3.5. Strength activity index

30

Table 4 and Fig. 7 show the compressive strength and the

strength activity indices of OPC and POFA mortars at the given
ages. The strength activity index of UPOFA and GPOFA was calculated based on the control sample (OPC mortar). The strength
activity index for 7 days of UPOFA and GPOFA were 97% and 75%
of OPC, respectively, which satised ASTM C 311-13 [22]. At the
age of 28 days, UPOFA exhibits 105% of strength activity index of
the OPC which is caused by the pozzolanic reaction. The data
clearly showed that UPOFA increased the compressive strength
even at early ages as compared to GPOFA. This may be due to the
neness of the particle and less amount of carbon content of
UPOFA. However, the activity index at 7 days is slightly lower than
the control sample. This may be due to dilution effect and delayed
onset of the pozzolanic reaction of Ca(OH)2 with POFA [25]. The
UPOFA mortar gives more percentage than the control sample at
28 days. Again, this showed that the packing effect of small particle
size and pozzolanic reaction was fully involved [26].
3.6. Heat of hydration test
The results of variation of the temperature versus time were
recorded for the different mortar types and presented in the
Table 5. A peak temperature of 50 C was recorded for OPC mortar
at 9 h while 34.1 C and 34.7 C were recorded at 11 h for GPOFA
and UPOFA, respectively. The development of temperature was
also obtained in the mid depth of mortar during the hydration process for all mortar samples and the results are shown in Fig. 8. It
has been observed that during the initial reading, the increase in
the temperature for the GPOFA and UPOFA mortar was almost similar. However, the comparison of the results of hydration temperature in the control sample and the other two types of mortar was
remarkably different. The use of POFA could successfully reduce
the total temperature rise compared to the normal OPC mortar
regardless the size of POFA. It has been researched that the neness

25
0

20

40

60

80

100

120

140

Fig. 8. The development of hydration temperature.

Table 5
The hydration temperature of OPC, GPOFA and UPOFA mortar.
Properties

OPC

GPOFA

UPOFA

Initial temperature (C)

Peak temperature (C)
Time since mixing to peak temperature (h)

28.6
50.0
9

28.7
34.1
11

29.4
34.7
11

of binder has an effect on the rate of heat development of samples

to some extent [10,26].
In the case of the reduction in hydration temperature, GPOFA
and UPOFA mortar performed more effectively than the OPC mortar, especially in the early steps where the peak in the temperature
was measured. This was also reported by Sata et al. [27] for the
normal concrete mixed with POFA. They have observed a
decreased of 30% temperature in mortar incorporating with 80%
POFA as compared to OPC mortar. The hydration temperature of
POFA mortar depends on the amount of calcium hydroxide
Ca(OH)2 in the hydration process of cement and reactivity of materials used. Hydration of cement was affected physically and chemically by adding other pozzolanic materials [12,2830].
Fig. 9 shows the compressive strength of OPC, GPOFA and
UPOFA mortars. The results show that the compressive strength
of mortar increased with the increasing age of curing. However,
using high volume UPOFA shows higher result compared to others
at all curing periods. This is due to the higher silica content after
50
45

110
UPOFA

GPOFA

Compressive strength (MPa)

105

OPC

Activity index (%)

100
95
90
85
80

OPC

80% UPOFA

80% GPOFA

40
35
30
25
20
15
10
5

75

70
7

14

Age (days)
Fig. 7. Strength activity index of mortar.

28

160

Time after casting (hr)

14
Age (days)

Fig. 9. Compressive strength of mortars.

28

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Nor Hasanah Abdul Shukor Lim et al. / Construction and Building Materials 93 (2015) 2934

(a)

(b)

Fig. 10. Field Emission Scanning Electron Microscope (FESEM) of (a) GPOFA and (b) UPOFA.

UPOFA mortar
Q
G
E

Q Quartz
E Ettringite
G Gypsum
Ca(OH)2 Calcium Hydroxide

Ca(OH)2

Q
E

Q
Ca(OH)2

GPOFA mortar

Q
G
E

Q
E

Ca(OH)2

Ca(OH)2

Fig. 11. XRD analysis of UPOFA and GPOFA mortars at 28 days.

the treatment process that helps the pozzolanic activities. The

hydration process was also examined by FESEM to study the paste
morphology.
Fig. 10 shows the FESEM for mortar containing GPOFA and
UPOFA. The gure shows that the ne UPOFA materials act both
as a binder and ller in the mortar [31,32]. Therefore, there are
fewer voids that can be observed in UPOFA specimens and more
calcium silicate hydrate crystal (CSH) which makes the mortar
more durable and denser.
Fig. 11 exhibits the XRD patterns for the UPOFA and GPOFA
mortar after 28 days curing. The amount of Ca(OH)2 in the pastes
point out its consumption in the pozzolanic reaction. More
Ca(OH)2 is consumed during pozzolanic reaction as the UPOFA contents increase because of the higher content of amorphous SiO2
available to react with Ca(OH)2. This reaction is more effective with
high amount of Ca(OH)2, which comes from the hydration process
of OPC. The addition of UPOFA resulted in an increase in CSH,
detected along the 2 Theta axis between 13.7 and 50.5 C of 2
Theta. The XRD graphs and SEM images conrmed this reaction.
In addition, the rate of pozzolanic reaction may be inuenced by
the neness of the UPOFA [33] (i.e., the neness of POFA affected
the production rate of CSH) [24]. Moreover, the ne POFA
provides more silica for pozzolanic reaction because it has a larger
surface area.

4. Conclusions
The following conclusions have been drawn from the experimental results of this research:
(1) High volume POFA with some modication can be used up
to 80% as cement replacement and achieve higher strength
than OPC mortar at a later age.
(2) Up to 105% of strength activity index can be achieved when
POFA is ground to a smaller size.
(3) The neness size of POFA which is less than 1 lm gives a
better effect to the mortar both as binder and ller.
(4) More than 80% nano palm oil fuel ash can be used to produce
mortar with an increased strength than normal mortar.
(5) High volume UPOFA reduces the heat of hydration of mortar
and can be used particularly for mass mortar application
where thermal cracking due to extreme heat rise is of great
concern.
Acknowledgements
The authors are grateful to the Ministry of Education, Malaysia
(MOE) and Research Management Centre (RMC), Universiti
Teknologi Malaysia (UTM) for nancial support under grant:

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Nor Hasanah Abdul Shukor Lim et al. / Construction and Building Materials 93 (2015) 2934

Q.J.130000.2522.03H36 and Q.J.130000.2509.06H56. The authors

are also thankful to the staff of Materials & Structures
Laboratory, Faculty of Civil Engineering for the facilities and support for the experimental work.
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