energies

Article
Influence of Conductive and Semi-Conductive
Nanoparticles on the Dielectric Response of Natural
Ester-Based Nanofluid Insulation
M. Z. H. Makmud 1,2, * ID
, H. A. Illias 1, *, C. Y. Chee 3 and M. S. Sarjadi 2
1 UM High Voltage Laboratory (UMHVL), Department of Electrical Engineering, Faculty of Engineering,
University of Malaya, 50603 Kuala Lumpur, Malaysia
2 Complex of Science and Technology, Faculty of Science and Natural Resources, Universiti Malaysia Sabah,
88400 Kota Kinabalu, Malaysia; msani@ums.edu.my
3 Department of Chemical Engineering, Faculty of Engineering, University of Malaya, 50603 Kuala Lumpur,
Malaysia; chingyc@um.edu.my
* Correspondence: mzhilmey@ums.edu.my (M.Z.H.M.); h.illias@um.edu.my (H.A.I.);
Tel.: +60-3-79674483 (H.A.I.)

Received: 26 December 2017; Accepted: 30 January 2018; Published: 2 February 2018

Abstract: Nowadays, studies of alternative liquid insulation in high voltage apparatus have
become increasingly important due to higher concerns regarding safety, sustainable resources and
environmentally friendly issues. To fulfil this demand, natural ester has been extensively studied
and it can become a potential product to replace mineral oil in power transformers. In addition,
the incorporation of nanoparticles has been remarkable in producing improved characteristics of
insulating oil. Although much extensive research has been carried out, there is no general agreement
on the influence on the dielectric response of base oil due to the addition of different amounts and
conductivity types of nanoparticle concentrations. Therefore, in this work, a natural ester-based
nanofluid was prepared by a two-step method using iron oxide (Fe2 O3 ) and titanium dioxide (TiO2 )
as the conductive and semi-conductive nanoparticles, respectively. The concentration amount of each
nanoparticle types was varied at 0.01, 0.1 and 1.0 g/L. The nanofluid samples were characterised by
visual inspection, morphology and the dynamic light scattering (DLS) method before the dielectric
response measurement was carried out for frequency-dependent spectroscopy (FDS), current-voltage
(I-V), and dielectric breakdown (BD) strength. The results show that the dielectric spectra and
I-V curves of nanofluid-based iron oxide increases with the increase of iron oxide nanoparticle
loading, while for titanium dioxide, it exhibits a decreasing response. The dielectric BD strength
is enhanced for both types of nanoparticles at 0.01 g/L concentration. However, the increasing
amount of nanoparticles at 0.1 and 1.0 g/L led to a contrary dielectric BD response. Thus, the results
indicate that the augmentation of conductive nanoparticles in the suspension can lead to overlapping
mechanisms. Consequently, this reduces the BD strength compared to pristine materials during
electron injection in high electric fields.

Keywords: natural ester; dielectric properties; electrical insulation; high voltage engineering

1. Introduction
Mineral-based insulation oil has been widely used in oil-immersed power transformers. The key
success of mineral oil is mainly due to its dual functionality as a good dielectric material with cooling
abilities and thee low cost associated with its availability. Today, the expansion of urbanisation
processes has led to ultra-high power demands and is consequently pushing power networks to their
limits. Hence, the failure rate of large power transformers increases, resulting in major environmental

Energies 2018, 11, 333; doi:10.3390/en11020333 www.mdpi.com/journal/energies

Energies 2018, 11, 333 2 of 12

damage and safety concerns. For instance, mineral-oil-based transformer explosions can cause toxicity
from the methane gas and oil spill onto the ground [1]. Hence, greater safety concerns have resulted in
the search for an alternative insulation oil. One of these is natural ester.
Natural ester (NE) is a new class of fully biodegradable dielectric insulation liquid that is
mainly developed from vegetable oils such as canola, rapeseed, soya beans, sunflower and palm
oil. Since the 1990s, work on suitability of NE as insulation for power industrial applications in natural
conditions, mixed with mineral oil or commercially produced as synthetic forms have been widely
reported [2–5]. For instance, NE can be synthesized into several derivatives with different molecular
structures and physiochemical properties. For example, increasing the length of the side branches of
chemically-modified alkyl ester of palm kernel oil will result in a higher breakdown strength compared
to mineral oil [6]. NE also has a higher molecular solubility and thereby can resist pressboard ageing
and moisture-rich environments [7,8].
Nowadays, the existence of nanotechnology has been utilized and the addition of nanoparticles
in insulating oil has produced a new remarkable material, known as nanofluids. NE-based nanofluids
have higher dielectric strength, cooling efficiency, and ability to withstand electrical discharges [9,10].
For instance, the discovered role of nanoparticles when being dispersed into base oil is to energise the
potential well. Therefore, it will trap the passing electrons and consequently lead to an enhancement
of dielectric strength [11]. In spite of this, it has been reported that the addition of conductive
nanoparticles in a certain amount reduces the dielectric strength of base oil [12–14]. When the number
of nanoparticles is increased, the collision rate between the particles increases due to Brownian motion,
but it appears as bridging between two conductors and could lead to breakdown [15]. The question is
why an identical phenomenon is also reported for semi-conductive and dielectric-based nanofluids [16].
It was believed that the enhancement of dielectric strength in nanofluids not only depends on the
intrinsic properties and interface regions formed between particles, as in solid phases [17–19]. However,
it strongly depends on the potential mobility of charged particles in nanofluid due to electric field
orientation. For instance, Ibrahim et al. [20] reported that the increasing number of conductive
nanoparticles (Fe2 NiO4 ) in the suspension will decrease the AC dielectric strength, and accumulated
particles were observed at the electrode under the DC electric field. However, there is no general
agreement regarding the influence of the conductivity and nanoparticle loading in nanofluid insulation.
Therefore, this work provides an opportunity to gain a better understanding of this matter in the fluid
phase by performing a comparative study using conductive and semi-conductive nanoparticles from
low to high amount of concentration using different dielectric measurement techniques.
A comparison of nanoparticle conductivity with different concentrations used to synthesise a
novel, natural, ester-based nanofluid intended as a high voltage insulation material is presented
in this work. The study compares the influence of the surface conductivity of nanoparticles and
the amount of concentration in relation to the dielectric responses of natural ester-based nanofluids
in frequency-dependent, current–voltage relation and breakdown strengths in high electric fields.
Iron oxide (Fe2 O3 ) and titanium dioxide (TiO2 ) were used in this work instead of other metal oxide
nanoparticles, e.g., magnesium oxide (MgO) and zinc oxide (ZnO) due to the latter particles showing
dissolution in the fluids with different pH values [21–23]. The results show that titanium dioxide
is more promising as a nanoparticle in natural ester for insulation purposes. The ability of TiO2
nanoparticles to remain as electron scavengers at varying concentrations is also discussed. A stable
suspension and particle size distribution after preparation is also described in this investigation.

2. Experimental

2.1. Materials
In this experiment, the natural ester used as the base oil was highly-refined, bleached, deodorised
palm oil (RBDPO), which was commercially obtained from Lam Soon Edible Oils Sdn. Bhd. (Shah
Alam, Malaysia). Iron oxide, Fe2 O3 ≥ 97% and titanium dioxide, TiO2 ≥ 99.5% were both obtained
Energies 2018, 11, 333 3 of 12

from Sigma Aldrich (St. Louis, MO, USA) in nanopowder form. They were used as conductive and
semi-conductive nanoparticles, respectively.

2.2. Sample Preparation

First, all materials were dried at a temperature of 80 ◦ C (for base oil) and 300 ◦ C (for nanoparticles)
in a thermal vacuum (90 kPa) chamber for one to two days. After drying and cooling-down processes,
nanoparticles were carefully added into 500 mL of natural ester (palm oil) with certain ratios as shown
in Table 1. In order to achieve a stable suspension, the sonication treatment was performed for 30 min
at room temperature using an ultrasonic bath (output power = 120 W, frequency = 40 kHz).

Table 1. Natural ester-based nanofluid formulations.

Amount of Nanoparticles [g/L]

Sample Abbreviation **
Iron Oxide Titanium Dioxide
NE - -
NE/Fe-a 0.01 -
NE/Fe-b 0.1 -
NE/Fe-c 1.0
NE/Ti-a - 0.01
NE/Ti-b - 0.1
NE/Ti-c - 1.0
** NE = Natural ester, Fe = Iron oxide, Ti = Titanium dioxide, a = 0.01 g/L, b = 0.1 g/L, c = 1.0 g/L.

2.3. Sample Characterisation Techniques

The nanofluid samples were characterized through three techniques: visual inspection,
morphology analysis and dynamic light scattering (DLS). Visual inspection is a technique for evaluating
the tendency of nanofluids to aggregate and eventually boost the sedimentation process with time.
After the natural ester-based nanofluid samples have been prepared, each sample was poured into
a cylindrical glass tube. The samples were left for 24 h without shaking to observe any changes
of the condition due to natural ambience before measurements were performed. The morphology
analysis was conducted using a scanning electron microscope (SEM) (Zeiss EVO® MA10, Oberkochen,
Germany). The nanofluid sample was deposited on the sticky tape of a SEM specimen holder and was
dried until solid particles were obtained. The dynamic light scattering (DLS) method was applied to
compare the average aggregate size of the nanoparticles at 0.01 g/L. Measurements were performed at
25 ◦ C using a Malvern Zetasizer (Malvern, UK).

2.4. Dielectric Response Measurements

Frequency dielectric spectroscopy (FDS) response and current-voltage (I-V) characteristic
measurements for the liquid under test were used in this work. The setup consists of two cylindrical
copper plates with a diameter of 25 mm and 100 µm gap distance. Both electrodes were fully immersed
in each nanofluid sample. For FDS measurement, a sinusoidal AC voltage of 0.5 Vrms was applied
to the test cell at room temperature with various frequencies, ranging between 0.1 Hz and 0.1 MHz.
The impedance results from the measurement were plotted in terms of dielectric constant, ε0 and
dielectric loss, ε00 . For I-V characteristic measurements, the parameters were adjusted using linear
sweep voltammetry (LSV) with a scan rate of 0.05 V/s and a step potential of 0.20 V. The applied DC
voltage was within a range of 1 to 10 V.
The dielectric breakdown voltage (BDV) of each sample was measured using an automated
test kit with a maximum applied voltage of 60 kV. The setup and procedure for each breakdown
of samples were in accordance with the ASTM D1816 standard. The gap space of the hemisphere
electrodes was set to 1.0 mm. The measured breakdown voltage of each sample was compared with
Energies 11, x333
2018, 11,
Energies 2018, FOR PEER REVIEW 4 of 12

the average breakdown voltage and Weibull distribution. The cumulative distribution function of
the average
Weibull breakdown
distribution voltage
for any and variable
random Weibull xdistribution.
is defined asThe cumulative distribution function of
Weibull distribution for any random variable x is defined as
f ( x ) = 1 − exp( − x / α ) β (1)
f (x) = 1 − exp( −x/α) β
(1)
where α is the scale parameter that corresponds to a probability of 63.2% and β is the shape parameter
that is αrelated
where to the
is the scale scattering
parameter ofcorresponds
that the data and to failure rate. To
a probability estimate
of 63.2% andthe
β isprobability of x as a
the shape parameter
function of breakdown voltage, the Weibull cumulative distribution function can be transformed
that is related to the scattering of the data and failure rate. To estimate the probability of x as a function into
a straight
of breakdownline voltage,
form as given by cumulative distribution function can be transformed into a straight
the Weibull
line form as given by    1  
ln ln  1   = β ln( x ) − β ln(α )
− f ( x )   = β ln( x ) − β ln(α)
(2)
ln ln 11− f (x)
(2)

Hence, ββ is directly represented by the slope of the line and α

α is evaluated from the y data that
intercepts with it.

3. Results

3.1. Sample Characterisation

3.1. Sample Characterisation Results
Results
Figure
Figure 11 shows
shows the
the natural
natural ester
ester samples
samples with
with different
different concentration
concentration levels
levels of
of iron
iron oxide
oxide and
and
titanium dioxide nanoparticles. When the nanoparticle concentration was increased,
titanium dioxide nanoparticles. When the nanoparticle concentration was increased, the nanofluid the nanofluid
samples
samples with
with iron
iron oxide
oxide took
took on
on aa dark
dark colour
colour while
while the
the nanofluid
nanofluid samples
samples with
with titanium
titanium dioxide
dioxide
became
became milky.
milky. Visual
Visual inspection
inspection was
was made
made atat the
the base
base of
of the
the glass
glass tube
tube to observe any
to observe any sedimentation
sedimentation
occurrence.
occurrence. IfIf sedimentation
sedimentationoccurred,
occurred,thethesample
sample was
wasrejected and
rejected a new
and sample
a new waswas
sample prepared. In this
prepared. In
work, no sedimentation occurred for 24 h, indicating that the dispersion of nanoparticles
this work, no sedimentation occurred for 24 h, indicating that the dispersion of nanoparticles within within the
sample is uniform
the sample is uniformandandthe sample waswas
the sample accepted for further
accepted experiments.
for further experiments.
NE/Ti - b
NE/Fe - a

NE/Ti - a
NE/Fe - b

NE/Ti - c
NE/Fe - c
NE

(a) (b)
Figure
Figure 1.
1. Samples
Samples of
of natural
natural ester
ester (NE)-based nanofluids; with:
(NE)-based nanofluids; with: (a)
(a) Iron oxide; (b)
Iron oxide; (b) Titanium
Titanium dioxide.
dioxide.

Figure 2a,b compares the distribution of the particles cross-sectional diameter and the volume
Figure 2a,b compares the distribution of the particles cross-sectional diameter and the volume
of the diversely-sized particle constituted. It can be seen that the iron oxide particles occupied a
of the diversely-sized particle constituted. It can be seen that the iron oxide particles occupied a
higher distribution compared to titanium dioxide. Therefore, it has a marked impact on the dielectric
higher distribution compared to titanium dioxide. Therefore, it has a marked impact on the dielectric
response of the suspension. Figure 2b shows the morphology of the formed particles from the
response of the suspension. Figure 2b shows the morphology of the formed particles from the titanium
titanium dioxide when a higher amount 1.0 g/L was deposited from the suspension. It was presumed
dioxide when a higher amount 1.0 g/L was deposited from the suspension. It was presumed that the
that the nanoparticles were dispersed homogenously due to only a small agglomeration size being
nanoparticles were dispersed homogenously due to only a small agglomeration size being observed.
observed. A Van Der Waals force from ultrasonication created a repulsive electrostatic potential
A Van Der Waals force from ultrasonication created a repulsive electrostatic potential between the electric
between the electric double layers (EDL) surrounding the particles [24]. Consequently, the fluid
double layers (EDL) surrounding the particles [24]. Consequently, the fluid stability was enhanced.
stability was enhanced.
 Energies 2018, 11, 333 5 of 12
Energies 2018, 11, x FOR PEER REVIEW 5 of 12

(a) (b)

2 µm
(c)
Figure 2. (a) Relative frequency distribution of nanoparticle size; (b) relative volume frequency
Figure 2. (a) Relative frequency distribution of nanoparticle size; (b) relative volume frequency
distribution of nanoparticle size and (c) Scanning electron microscope (SEM) micrograph and the
distribution of nanoparticle size and (c) Scanning electron microscope (SEM) micrograph and the
arrows point to the nanoparticle agglomeration.
arrows point to the nanoparticle agglomeration.

3.2. Frequency Dielectric Response (FDS) Results

3.2. Frequency Dielectric Response (FDS) Results
Figure 3a,b shows the measured dielectric spectroscopy at different frequencies of natural ester-
Figure 3a,b shows the measured dielectric spectroscopy at different frequencies of natural
based nanofluid samples. It can be seen clearly that the dielectric constant, ′ of NE/Fe a, b, and c
ester-based nanofluid samples. It can be seen clearly that the dielectric constant, ε0 of NE/Fe a, b, and c
exhibits slightly stronger frequency-dependency with an increase of iron oxide concentration at 0.01,
exhibits slightly stronger frequency-dependency with an increase of iron oxide concentration at 0.01,
0.1 and 1.0 g/L, respectively. Surprisingly, the dielectric constant, ′ of the NE/Ti shows quite
0.1 and 1.0 g/L, respectively. Surprisingly, the dielectric constant, ε0 of the NE/Ti shows quite different
different trends, especially for the concentration amount of titanium dioxide at 0.1 and 1.0 g/L.
trends, especially for the concentration amount of titanium dioxide at 0.1 and 1.0 g/L. Although the
Although the presences of the hydroxyl group on the surface of particles or the impurities, such as
presences of the hydroxyl group on the surface of particles or the impurities, such as polar species,
polar species, can affect the polarization, it can be minimized by pre-heat treatment during sample
can affect the polarization, it can be minimized by pre-heat treatment during sample preparation [25,26].
preparation [25,26]. Therefore, the apparent polarization in this study is the summation of the
Therefore, the apparent polarization in this study is the summation of the polarization of the base
polarization of the base oil, inner polarization of nanoparticles and orientation polarization of
oil, inner polarization of nanoparticles and orientation polarization of charged nanoparticles as polar
charged nanoparticles as polar molecules due to Miao et al. [27]. Since the electrical properties of iron
molecules due to Miao et al. [27]. Since the electrical properties of iron oxide are more conductive
oxide are more conductive than titanium dioxide, it can be more easily charged and polarized than
than titanium dioxide, it can be more easily charged and polarized than titanium dioxide when being
titanium dioxide when being dispersed in natural ester. The mobility of charged particles may also
dispersed in natural ester. The mobility of charged particles may also influence the polarization process
influence the polarization process at low frequencies.
at low frequencies.
Figure 4a,b shows the measured dielectric loss ε00 as a function of frequency for natural ester-based
nanofluid samples with conductive and semi-conductive nanoparticles. At very low frequencies,
natural ester-based nanofluid samples with conductive, NE/Fe a, b and c exhibit higher dielectric loss
ε00 than the samples with semi-conductive nanoparticles, NE/Ti a, b, and c. At higher frequencies,
relaxation spectra are dominant and clearly visible for all samples. This is associated with a descend
Energies 2018, 11, 333 6 of 12

conduction mechanism due to the low mobility of charge carriers, which is likely to be suppressed
by a high frequency field. However, at lower frequencies (0.1 Hz to 10 Hz), when nanoparticles were
dispersed in a base oil, free charges in the natural ester are trapped by nanoparticles. This hinders
charge carriers to move between two electrodes and consequently, the dielectric loss decreases.
However, as the concentration(a) of nanoparticles is higher in the sample, the(b)probability of the electric
double layer (EDL) region overlapping is higher, producing a higher conductive region along the
Figure 3. Dielectric constant ′ as a function of frequency for natural ester-based nanofluids with: (a)
natural ester ions.
Conductive The effect
nanoparticles; (b)on the conductive
Semi-conductive path of the overlapping EDL is more sensitive in
nanoparticles.
highly-conductive
Energies 2018, 11, x FORnanoparticles,
PEER REVIEW which can be seen from the response of NE/Fe-c in Figure 4a. 6 of 12
Figure 4a,b shows the measured dielectric loss ″ as a function of frequency for natural ester-
based nanofluid samples with conductive and semi-conductive nanoparticles. At very low
frequencies, natural ester-based nanofluid samples with conductive, NE/Fe a, b and c exhibit higher
dielectric loss ″ than the samples with semi-conductive nanoparticles, NE/Ti a, b, and c. At higher
frequencies, relaxation spectra are dominant and clearly visible for all samples. This is associated
with a descend conduction mechanism due to the low mobility of charge carriers, which is likely to
be suppressed by a high frequency field. However, at lower frequencies (0.1 Hz to 10 Hz), when
nanoparticles were dispersed in a base oil, free charges in the natural ester are trapped by
nanoparticles. This hinders charge carriers to move between two electrodes and consequently, the
dielectric loss decreases. However, as the concentration of nanoparticles is higher in the sample, the
probability of the electric (a) double layer (EDL) region overlapping is higher, (b) producing a higher
conductive region along the natural ester ions. The effect on the conductive path of the overlapping
EDL Figure
is more3. Dielectric constant ′ as a functionnanoparticles,
of frequency forwhich
naturalcan
ester-based
be seennanofluids
the with: (a)
Figure 3. sensitive
Dielectricin highly-conductive
constant ε0 as a function of frequency for from
natural ester-based response
nanofluids with: of
Conductive
NE/Fe-c
(a) in Figure
Conductivenanoparticles;
4a. (b) (b)
nanoparticles; Semi-conductive
Semi-conductivenanoparticles.
nanoparticles.

Figure 4a,b shows the measured dielectric loss ″ as a function of frequency for natural ester-
based nanofluid samples with conductive and semi-conductive nanoparticles. At very low
frequencies, natural ester-based nanofluid samples with conductive, NE/Fe a, b and c exhibit higher
dielectric loss ″ than the samples with semi-conductive nanoparticles, NE/Ti a, b, and c. At higher
frequencies, relaxation spectra are dominant and clearly visible for all samples. This is associated
with a descend conduction mechanism due to the low mobility of charge carriers, which is likely to
be suppressed by a high frequency field. However, at lower frequencies (0.1 Hz to 10 Hz), when
nanoparticles were dispersed in a base oil, free charges in the natural ester are trapped by
nanoparticles. This hinders charge carriers to move between two electrodes and consequently, the
dielectric loss decreases. However, as the concentration of nanoparticles is higher in the sample, the
probability of the electric (a) double layer (EDL) region overlapping is higher, (b) producing a higher
conductive region along the natural ester ions. The effect on the conductive path of the overlapping
Figure
Figure 4.4. Dielectric
Dielectricloss
loss″ ε00as as
a function of of
a function frequency for for
frequency natural ester-based
natural nanofluids
ester-based with:with:
nanofluids (a)
EDLConductive
is more sensitive in highly-conductive
nanoparticles; (b) Semi-conductive
nanoparticles,
nanoparticles.
which can be seen from the response of
(a) Conductive nanoparticles; (b) Semi-conductive nanoparticles.
NE/Fe-c in Figure 4a.
3.3.
3.3. Current-Voltage
Current-Voltage (I-V)
(I-V)Results
Results
Figure
Figure5a,b
5a,brepresent
representthe I-VI-V
the curves of natural
curves ester-based
of natural nanofluids
ester-based with conductive
nanofluids with conductiveand semi-
and
conductive nanoparticles. It was found that the I-V results show that the conduction
semi-conductive nanoparticles. It was found that the I-V results show that the conduction current increases
current
gradually
increases with the voltage
gradually andvoltage
with the verifiedand
thatverified
the samples havesamples
that the a resistance
havemode that is similar
a resistance mode thatto theis
behaviour of nanofluids [28]. The resistivity value for pure natural ester is high, at 3.08
similar to the behaviour of nanofluids [28]. The resistivity value for pure natural ester is high, GΩ·m. Under
the applied
at 3.08 GΩDC·m. electric
Underfield,
the the number
applied DCofelectric
electrons as charge
field, carriersofincreases
the number electronsin as
thecharge
channelcarriers
above
the threshold
increases voltage.
in the Thus,
channel the conduction
above the thresholdcurrent increases
voltage. in symmetrical
Thus, the conduction non-linear
currentfashion
increaseswithin
the voltage. At a low loading of nanoparticles, both the NE/Fe and NE/Ti samples
symmetrical non-linear fashion with the voltage. At a low loading of nanoparticles, both the NE/Feshow a reduction
of charge
and NE/Timobility
samplesinshow
the DC electric field.
a reduction At this
of charge critical in
mobility interface
the DC distance, it shows
electric field. a trapping
At this charge
critical interface
distance, it shows a trapping charge ability through a polarization and charge induction mechanism,
(a) (b)
consequently enhancing the insulation properties [29]. However, when the particle loading increases
in the suspension,
Figure 4. Dielectric loss ″volume
a higher of particles
as a function in conjunction
of frequency for naturalwith electricnanofluids
ester-based field orientation
with: (a) may
deteriorate the critical
Conductive interface
nanoparticles; (b)distance betweennanoparticles.
Semi-conductive inter-particles. Therefore, it leads to a new condition

3.3. Current-Voltage (I-V) Results

Figure 5a,b represent the I-V curves of natural ester-based nanofluids with conductive and semi-
conductive nanoparticles. It was found that the I-V results show that the conduction current increases
gradually with the voltage and verified that the samples have a resistance mode that is similar to the
Energies 2018, 11, x FOR PEER REVIEW 7 of 12
Energies 2018, 11, x FOR PEER REVIEW 7 of 12
ability through a polarization and charge induction mechanism, consequently enhancing the
ability
insulationthrough a polarization
properties and when
[29]. However, charge
theinduction mechanism,
particle loading increasesconsequently enhancing
in the suspension, the
a higher
insulation
volume of properties
Energies 2018,
particles in[29].
11, 333 However,
conjunction when
with the particle
electric loading increases
field orientation in the suspension,
may deteriorate a higher
7 of
the critical interface 12
volume
distanceof particles
between in conjunctionTherefore,
inter-particles. with electric fieldtoorientation
it leads may deteriorate
a new condition where thethe criticalproperties
intrinsic interface
distance
(particle between inter-particles. Therefore, it leads to a new condition where the intrinsic properties
where thesurface
intrinsicconductivity) are moresurface
properties (particle dominant. It can be seen
conductivity) fromdominant.
are more the I-V result that
It can bethe
seennatural
from
(particle
ester-basedsurface conductivity)
nanofluid are more
containing dominant. Itnanoparticles
semi-conductive can be seen from
is the I-Vespecially
reduced result thatfor theNE/Ti-b
natural
the I-V result that the natural ester-based nanofluid containing semi-conductive nanoparticles is
ester-based
and NE/Ti-c. nanofluid
This for containing
is due to the semi-conductive
larger amount nanoparticles is reduced especially for NE/Ti-b
reduced especially NE/Ti-b and NE/Ti-c. Thisofis titanium
due to thedioxide in natural
larger amount ester, which
of titanium could
dioxide in
and NE/Ti-c.
improve the This
charge is due to
trapping the
and larger amount
increase the of
surfacetitanium dioxide
resistance. in natural
However, for ester,
natural which could
ester-based
natural ester, which could improve the charge trapping and increase the surface resistance. However,
improve
nanofluids thewith
charge irontrapping
oxide, andincorporation
the increase the surface resistance.
of conductive However, for
nanoparticles naturalamounts
in larger ester-based
has
for natural ester-based nanofluids with iron oxide, the incorporation of conductive nanoparticles
nanofluids
modified with
the iron
tube–tube oxide, the
contact incorporation
resistance, of
which conductive
improved nanoparticles
the conduction in larger amounts
mechanism of has
the
in larger amounts has modified the tube–tube contact resistance, which improved the conduction
modified
nanofluid. the
This tube–tube
proposed contact resistance,
mechanism also can which
be improved
attributed as the
the conduction
percolation mechanism
threshold in of the
nanofluid
mechanism of the nanofluid. This proposed mechanism also can be attributed as the percolation
nanofluid.
cases. This proposed mechanism also can be attributed as the percolation threshold in nanofluid
threshold in nanofluid cases.
cases.

(a) (b)
(a) (b)
Figure 5.
Figure 5. I-V
I-V curves
curves of
of natural
natural ester-based
ester-based nanofluids
nanofluids with:
with: (a)
(a) Conductive
Conductive nanoparticles;
nanoparticles; (b)
(b) Semi-
Semi-
Figure 5. I-V
conductive curves of natural ester-based nanofluids with: (a) Conductive nanoparticles; (b) Semi-
nanoparticles.
conductive nanoparticles.
conductive nanoparticles.
3.4. Dielectric Breakdown Voltage (BDV) Results
3.4. Dielectric Breakdown Voltage (BDV) Results
3.4. Dielectric Breakdown Voltage (BDV) Results
The measured dielectric breakdown voltage (BDV) for each sample is presented in Figure 6. The
The measured dielectric breakdown voltage (BDV) for each sample is presented in Figure 6.
The measured
breakdown voltagedielectric
of naturalbreakdown voltage
ester without (BDV) for as
nanoparticles, each sample by
indicated is presented in Figure
NE, is around 6. The
31 kV. The
The breakdown voltage of natural ester without nanoparticles, as indicated by NE, is around 31 kV.
breakdown voltage of natural ester without nanoparticles, as indicated by NE, is around
BDV of NE/Fe-a and NE/Ti-a with 0.01 g/L amount of conductive, semi-conductive nanoparticles 31 kV. The
The BDV of NE/Fe-a and NE/Ti-a with 0.01 g/L amount of conductive, semi-conductive nanoparticles
BDV of NE/Fe-a
respectively and NE/Ti-a
is higher than thewith
pure0.01 g/L amount
sample, of conductive,
NE. However, the BDVsemi-conductive nanoparticles
of NE-based nanofluids with
respectively is higher than the pure sample, NE. However, the BDV of NE-based nanofluids with
respectively is higher than the pure sample, NE. However, the BDV of NE-based nanofluids
conductive nanoparticles shows a higher BDV than the NE pure sample at lower amounts only. The with
conductive nanoparticles shows a higher BDV than the NE pure sample at lower amounts only.
conductive nanoparticles
dielectric breakdown shows
voltage a higher
of NE/Fe BDV than
nanofluids the NE pure
decreases sample at
significantly lower
with the amounts only.
increasing The
amount
The dielectric breakdown voltage of NE/Fe nanofluids decreases significantly with the increasing
dielectric breakdown
of conductive voltage of NE/Fe nanofluids decreases significantly with the increasing amount
nanoparticles.
amount of conductive nanoparticles.
of conductive nanoparticles.

Figure 6. Dielectric breakdown voltage of natural ester-based nanofluids.

voltage of
Figure 6. Dielectric breakdown voltage of natural
natural ester-based
ester-based nanofluids.
nanofluids.
Energies 2018, 11, 333 8 of 12
Energies 2018, 11, x FOR PEER REVIEW 8 of 12

The average breakdown

breakdown voltage does not not represent
represent the probability
probability that thethe insulation
insulation willwill break
break
down
down when
when being
being stressed
stressed with
with high
high electric
electric fields.
fields. Thus,
Thus, the
the Weibull
Weibull distribution
distribution was appliedapplied as a
statistical tool
tooltotoprovide
provide thethe degree
degree of withstanding
of withstanding capability
capability of theofsamples.
the samples.
Since theSince the voltage
lowest lowest
voltage
at whichatbreakdown
which breakdown
will occurwill occur
is the is the
main mainfor
interest interest for insulation
insulation applications,
applications, it is important
it is important to observe
to
theobserve theoflower
lower tail tail of the
the Weibull Weibull slopes.
distribution distribution slopes.
Referring Referring
to Figure 7a,b,toitFigure 7a,b, it
is observed is observed
that the range
that
of thethe range of the
breakdown breakdown
probability probability
of the of the natural
natural ester-based ester-based
nanofluid nanofluid
with iron oxide with iron oxide
is relatively is
lower
relatively lower for
for the NE/Fe-b andthe NE/Fe-bsamples
NE/Fe-c and NE/Fe-c samples
compared compared
to the to theester.
pure natural pureThenatural
rangeester. The range
of breakdown
of breakdown
probability probability
of the of the natural
natural ester-based ester-based
nanofluid nanofluid
with titanium withis more
dioxide titanium dioxide than
pronounced is more
the
pronounced
pure natural than
ester,the pure natural
especially for theester, especially
NE/Ti-b for the NE/Ti-b
and NE/Ti-c samples.and NE/Ti-c samples.

(a) (b)
Figure 7. Weibull distribution of dielectric breakdown of natural ester-based nanofluids with: (a)
Figure 7. Weibull distribution of dielectric breakdown of natural ester-based nanofluids with:
Conductive nanoparticles; (b) Semi-conductive nanoparticles.
(a) Conductive nanoparticles; (b) Semi-conductive nanoparticles.

4. Discussion
4. Discussion
Electrical breakdown in a liquid dielectric is initiated by the streamer formation between two
Electrical breakdown in a liquid dielectric is initiated by the streamer formation between two
electrodes when the electric field intensity exceeds their threshold level. At this level, the molecules
electrodes when the electric field intensity exceeds their threshold level. At this level, the molecules of
of the liquid are ionized and more ions and electrons are created, forming a conductive path known
the liquid are ionized and more ions and electrons are created, forming a conductive path known as a
as a streamer. After a streamer is formed, it tends to elongate and transverse in the dielectric liquid
streamer. After a streamer is formed, it tends to elongate and transverse in the dielectric liquid from the
from the point of initiation towards the lowest potential in the system, which is usually the grounded
point of initiation towards the lowest potential in the system, which is usually the grounded electrode.
electrode. When the streamer reaches the grounded electrode, it forms a bridge or short circuit
When the streamer reaches the grounded electrode, it forms a bridge or short circuit between the two
between the two electrodes. Eventually, a current or arc flows through it, which causes a dielectric
electrodes. Eventually, a current or arc flows through it, which causes a dielectric breakdown [30].
breakdown [30].
It is known that refined, bleached, deodorised palm oil (RBDPO) is a low melting liquid fraction
It is known that refined, bleached, deodorised palm oil (RBDPO) is a low melting liquid fraction
of natural ester, which consists of oleic acid (C18:1) at 48% due to refining and good bleaching
of natural ester, which consists of oleic acid (C18:1) at 48% due to refining and good bleaching
processes [31]. Oleic acid acts as a natural surfactant when metal oxide nanoparticles are dispersed into
processes [31]. Oleic acid acts as a natural surfactant when metal oxide nanoparticles are dispersed
a base oil during the sample preparation process. A mechanically-stable natural ester-based nanofluid
into a base oil during the sample preparation process. A mechanically-stable natural ester-based
sample is obtained when oleic acid is chemisorbed as carboxylate on the nanoparticle surface. Hence,
nanofluid sample is obtained when oleic acid is chemisorbed as carboxylate on the nanoparticle
the interfacial zone of the nanofluid as a solid–liquid suspension is enhanced [32]. The role of the
surface. Hence, the interfacial zone of the nanofluid as a solid–liquid suspension is enhanced [32].
interfacial zone in a nanofluid is to create intermolecular forces, which keeps the molecules from each
The role of the interfacial zone in a nanofluid is to create intermolecular forces, which keeps the
other according to the Van Der Waals theorem. As a result, the nanoparticle consists of two layers,
molecules from each other according to the Van Der Waals theorem. As a result, the nanoparticle
the affected and aligned layers, which are difficult to polarize, trapping charges and slowing down the
consists of two layers, the affected and aligned layers, which are difficult to polarize, trapping charges
electron mobility, as suggested by Mansour et al. [33]. For low volumes (0.01 g/L) of nanoparticles in
and slowing down the electron mobility, as suggested by Mansour et al. [33]. For low volumes
natural ester, the interfaces have a large space to form an efficient distance of double layers. This is
(0.01 g/L) of nanoparticles in natural ester, the interfaces have a large space to form an efficient
a possible mechanism explaining the reduction of the total amount of polarization for both types
distance of double layers. This is a possible mechanism explaining the reduction of the total amount
of nanoparticles, resulting in a decrease of dielectric constant. The aligned layers also create a rigid
of polarization for both types of nanoparticles, resulting in a decrease of dielectric constant. The
aligned layers also create a rigid intermolecular structure that traps electron and ion mobility between
 Energies2018,
Energies 2018,11,
11,333
x FOR PEER REVIEW 9 9ofof1212

interparticle zones, resulting in a decrease in the conduction current and consequently an increase in
intermolecular structure that
the dielectric breakdown traps electron and ion mobility between interparticle zones, resulting in a
voltage.
decreaseOninthe theother
conduction
hand, current
for higherand amounts
consequently an increase in(0.1
of nanoparticles the and
dielectric breakdown
1.0 g/L), voltage.
the interparticle
On the
distance other hand,
decreases, for higher
reducing amounts
the efficient widthof nanoparticles
of double layers, (0.1 and
and overlapping
1.0 g/L), thewill interparticle
potentially
distance
occur. In decreases,
conjunction reducing
with thethe applied
efficient electric
width of double
field, layers,can
particles andbeoverlapping
easily charged willandpotentially
move to
occur.
bridging the flow of electrons [20]. For highly-conductive nanoparticles, such as iron oxide, when to
In conjunction with the applied electric field, particles can be easily charged and move the
bridging
amountthe flow of ester
in natural electrons [20].a smaller
is high, For highly-conductive
interparticle distancenanoparticles, such
affects the as iron
electric oxide,
field when the
enhancement.
amount
This isindue natural
to the ester is high,
effect a smaller interparticle
of nanoparticle distance affects
surface conductivity the more
being electricdominant.
field enhancement.
For semi-
This is due to and
conductive the effect of nanoparticle
dielectric nanofluids, surface conductivity
reduction being more
and overlapping ofdominant. For semi-conductive
the interfacial zone space does
and
notdielectric
affect thenanofluids, reductionmuch
dielectric response and overlapping
because theyofcan theattract
interfacial zoneelectrons
and trap space does in not affecttraps,
shallow the
dielectric
as well as response
having very muchlow because they canvalues
conductivity attract[20,34].
and trap electrons in shallow
Nevertheless, traps,exist
if impurities as well
on theas having
particle
very low conductivity
surface, they play anvalues [20,34].
important roleNevertheless,
in the mechanism,if impurities exist on
increasing thethe particleconductivity
electrical surface, they of play
the
anbase
important
materialrole in the mechanism, increasing the electrical conductivity of the base material [25].
[25].
Figure
Figure8 illustrates
8 illustrates the electric displacement
the electric field and
displacement current
field and density
currentdistributions in the nanofluid
density distributions in the
with the influence
nanofluid with the of influence
nanoparticle properties using
of nanoparticle finite element
properties analysis
using finite element(FEA) between
analysis (FEA) twobetween
plane
electrodes.
two planeWhen the electrical
electrodes. When the properties
electricalofproperties
a nanoparticle are different are
of a nanoparticle from the basefrom
different oil, the
the electric
base oil,
field
the intensity surrounding
electric field intensitythe nanoparticle
surrounding thewill be distorted.
nanoparticle For
will beinstance as described
distorted. For instance in [20], a larger
as described
distortion of the distortion
in [20], a larger electric field results
of the in afield
electric higher magnitude
results in a higherof the electric field
magnitude of theonelectric
the nanoparticle
field on the
interface,
nanoparticlesubsequently
interface, exerting
subsequentlya force that attracts
exerting a forcefree thatelectrons. Also,
attracts free a high Also,
electrons. current density
a high at
current
density
the at the nanoparticle
nanoparticle surface shows surface shows that
that streamer streamer can
penetration penetration
occur morecaneasily
occurwith
morethe easily with of
presence the
presence
highly of highlynanoparticle
conductive conductive in nanoparticle
natural ester.in natural
As can ester.
be seen Asfrom
can be seen8a,b,
Figure fromnatural
Figure ester-based
8a,b, natural
ester-based
nanofluids withnanofluids
iron oxidewith haveiron
higheroxide have higher
magnitudes magnitudes
of current densityofcompared
current density
to titaniumcompared
dioxide,to
titanium
which can dioxide, whicha can
easily initiate easily initiate
breakdown in higha breakdown
electric fields. in high electric fields.

(a) (b)
Figure8. 8.
Figure TheThe magnitude
magnitude of surface
of surface current
current densitydensity on a nanoparticle:
on a nanoparticle: (a) Conductive;
(a) Conductive; (b) Semi-
(b) Semi-conductive.
conductive.
5. Conclusions
5. Conclusions
In this work, investigation of the influence of nanoparticles, iron oxide and titanium dioxide on
In this work,
the dielectric responseinvestigation of the influence
of natural ester-based of nanoparticles,
nanofluid ironsuccessfully
insulation was oxide and titanium dioxide
performed. Some on
the dielectric response of natural ester-based
meaningful findings are summarized as follows: nanofluid insulation was successfully performed. Some
meaningful findings are summarized as follows:
1. Natural ester, such as palm oil, which consists of natural oleic acid as a substantial content,
1. produces
Natural aester,
stablesuch as palm
nanofluid oil, which
suspension whenconsists of natural
dispersed oleicoxide
with metal acid nanoparticles.
as a substantial content,
Oleic acid
produces
plays a stable nanofluid
an important role as an suspension when dispersed
artificial surfactant, with metal
which enhances the oxide nanoparticles.
suspension Oleic
stability and
acid plays an important
avoids agglomeration. role as an artificial surfactant, which enhances the suspension stability
2. and
At avoids
0.01 agglomeration.
g/L concentration of nanoparticles within natural ester, the effect of the interfacial zone
2. wasAt 0.01
dominant and a largeof
g/L concentration nanoparticles
space within natural ester,
for rigid intermolecular forcesthe
waseffect of therequiring
created, interfacial zone
more
was dominant and a large space for rigid intermolecular forces was created, requiring more
Energies 2018, 11, 333 10 of 12

energy to break up. This behaviour was shown through the reduction of dielectric loss and the
enhancement of dielectric strength for both types of nanoparticles.
3. When the concentration of nanoparticles within natural ester was increased to 0.1 and 1.0 g/L,
respectively, the dielectric response of nanofluids became more dependent on the nanoparticle
properties (in this case, surface conductivity). Since iron oxide is highly conductive compared
to titanium dioxide, the enhancement of the polarization and conduction current was observed
with increasing concentration of conductive nanoparticles. This has also led to the reduction of
dielectric breakdown voltage.

Acknowledgments: The authors thank the University of Malaya, Malaysia and Ministry of Higher Education,
Malaysia for supporting this work through HIR research grant (grant number: HIR H-16001-D00048), Postgraduate
Research Funds (grant number: PPP PG236-2016A) and Fundamental Research Grant Scheme (grant number:
FRG0413-SG-1/2015).
Author Contributions: M. Z. H. Makmud, H. A. Illias, and C. Y. Chee designed the study. M. Z. H. Makmud
performed the experiment, analyse the results and wrote the paper with the feedback from H. A. Illias, C. Y. Chee
and M. S. Sarjadi.
Conflicts of Interest: The authors declare no conflict of interest.

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