Nanomaterials 12 02105 v2

nanomaterials
Article
Effect of Conducting, Semi-Conducting and Insulating
Nanoparticles on AC Breakdown Voltage and Partial Discharge
Activity of Synthetic Ester: A Statistical Analysis
Hocine Khelifa * , Abderrahmane Beroual and Eric Vagnon
Ecole Centrale de Lyon, University of Lyon, Ampère CNRS UMR5005, 69130 Ecully, France;
abderrahmane.beroual@ec-lyon.fr (A.B.); eric.vagnon@ec-lyon.fr (E.V.)
* Correspondence: hocine.khelifa@ec-lyon.fr
Abstract: This paper is aimed at studying the influence of conducting (Fe3 O4 ), semi-conductive
(ZnO), and insulating (ZrO2 , SiO2 , and Al2 O3 ) nanoparticles (NPs) at various concentrations on
the AC dielectric strength of MIDEL 7131 synthetic ester (SE) and partial discharges activity. First,
a detailed and improved procedure for preparing nanofluids (NFs) in five concentrations ranging
from 0.1 g/L to 0.5 g/L is presented, including high-speed agitation and ultrasonication. Then, the
long-term stability is checked based on zeta potential analysis. After preparing and characterizing
the NF samples, the following step is to measure their AC breakdown voltage (BDV). Due to the
limitation of the high voltage supply (Baur system), the tests are performed according to IEC 60156
standard (2.5 mm gap distance) only with ZnO, ZrO2 , and SiO2 NPs, and for comparison, tests are
executed for all considered NPs with an electrodes gap of 2 mm. It is shown that the addition of Fe3 O4
(20 nm), ZnO (25 nm), ZrO2 (20–30 nm), SiO2 (10–20 nm), Al2 O3 (20–30 nm), and Al2 O3 (50 nm) NPs
improves the dielectric strength of synthetic ester upon an optimal concentration which gives the
Citation: Khelifa, H.; Beroual, A.; highest AC BDV. SiO2 (10–20 nm) and Al2 O3 (20–30 nm) manifest their best improvement at 0.3 g/L,
Vagnon, E. Effect of Conducting, while for the other NFs, the best improvement is observed at 0.4 g/L. Further, the Anderson–Darling
Semi-Conducting and Insulating goodness-of-fit test is performed on the experimental data to check their conformity with the Extreme
Nanoparticles on AC Breakdown value (EV), normal, and Weibull distributions; the normal and EV fit curves are plotted and used
Voltage and Partial Discharge
to evaluate the breakdown voltages at probabilities of 1%, 10%, and 50%. It is shown that the AC
Activity of Synthetic Ester: A
breakdown voltage outcomes for most investigated nanofluids mostly obey the three EV, normal, and
Statistical Analysis. Nanomaterials
Weibull distributions. Then, the best combinations (nature of NP and optimal concentration), namely
2022, 12, 2105. https://doi.org/
Fe3 O4 (20 nm, 0.4 g/L), Al2 O3 (20–30 nm, 0.3 g/L), and Al2 O3 (50 nm, 0.4 g/L) NPs, that highly
10.3390/nano12122105
enhance the AC BDV of SE are chosen for a partial discharge activity investigation and comparison
Academic Editor: Sergio Brutti with pure SE. It is shown that the addition of those NPs significantly reduces the activity of partial
Received: 20 April 2022 discharges compared to pure SE.
Accepted: 17 June 2022
Published: 19 June 2022 Keywords: nanofluids; synthetic ester; oxide nanoparticles; AC breakdown voltage; partial
discharges; statistical analysis; extreme value distribution; normal and Weibull distributions
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with regard to jurisdictional claims in
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iations.
1. Introduction
Nowadays, nanotechnology has emerged as one of the most exciting and advanc-
ing areas in science and engineering. Most academic centers and industries around the
Copyright: © 2022 by the authors. globe have been occupied in focusing on nanoscale research as a part of miniaturiza-
Licensee MDPI, Basel, Switzerland. tion/proficiency in devices. As an indication, biological and medical communities exploit
This article is an open access article the properties of nanomaterials for a variety of applications under the terms nanobiology
distributed under the terms and
and nanomedicine [1,2]. The size of biological structures or molecules is quite close to
conditions of the Creative Commons
those materials. Therefore, they could add functions to those structures/molecules. This
Attribution (CC BY) license (https://
immense integration allows reliable diagnostic or rapid drug administration tools [3,4].
creativecommons.org/licenses/by/
Moreover, electronic chips or integrated circuits are already nano-scaled component-based
4.0/).
Nanomaterials 2022, 12, 2105. https://doi.org/10.3390/nano12122105 https://www.mdpi.com/journal/nanomaterials

Nanomaterials 2022, 12, 2105 2 of 25
and extensively use nanotechnology [5]. Thanks to the emergence of nanotechnology in

energy conversation, today’s solar panels yield twice as much energy [5,6].
An innovative concept termed “Nanofluids” (NFs) in science and engineering refers
to the exploitation of the unique properties of nanoparticles for various applications. Chen
et Eastman. [7] introduced it in the late twentieth century. The nanoparticles (NPs) are
homogeneously mixed up within a base liquid with a proper technic. A typical example of
a nanofluid is the iron oxide (Fe3 O4 ) nanoparticles dispersed in a host liquid, such as water.
In the beginning, it represented the best belief for heat transfer enhancement [7]; this was
proven so far, and more recently, the attention has been paid to how better the dielectrics
liquids would be in the presence of these particles for insulation applications and how they
affect their properties [8–16]. Among these properties, the breakdown voltage (BDV) was
considered as the essential property to be taken into consideration. Thus, recent years have
seen a rise in the number of related publications.
Olmo et al. [17] reported that the addition of TiO2 NPs (10–20 nm) improves the AC
breakdown voltage of natural ester (NE) by 33.2% at a concentration of 0.5 g/L, while
with the other concentrations, the enhancements are 25.8%, 30.4%, 21.6%, and 7.6% for
the concentration of 0.1, 0.2, 0.7, and 1 g/L, respectively. Peppas et al. [13] and Khaled
and Beroual [15,16] found a similar tendency with Fe3 O4 , Al2 O3 , and SiO2 nanofluids at
different concentrations (0.05 to 0.5 g/L). With equal spherical particle sizes (50 nm), Khaled
and Beroual [16] investigated the effect of conductive (Fe3 O4 ) and insulation nanoparticles
(Al2 O3 and SiO2 ) on the breakdown voltage of synthetic ester (SE)-based nanofluids. They
found that SE-based NF with Fe3 O4 enhances the BDV about 48% against 25% and 32%
with Al2 O3 and SiO2 , respectively, compared to the host liquid. They reported that the
insulation nanoparticles give somewhat the same improvement; conductive nanoparticles
provide the best enhancement. Those results put forward the possible implications of
electrical conductivity on the breakdown mechanisms. Hussain et al. [8] examined the
effect of adding magnetic NPs, namely iron oxide (Fe3 O4 ), cobalt oxide (Co3 O4 ), and iron
phosphide (Fe3 P), on the insulation performances of synthetic and natural esters. They
show that these NPs enhance the dielectric strength of both types of liquids. Furthermore,
the Fe3 P NFs show the best improvements at an optimal concentration of 0.02 g/L. Those
enhancements are 20.2% and 31.4% for SE and NE-based NFs, respectively.
Hwang et al. [11] explained the AC BDV improvement via electron trapping as a
possible mechanism based on the relaxation time constant (τr ). This mechanism nicely
explains the enhancement of base liquid’s insulating performances with addressed conduc-
tive NPs (Fe3 O4 ), but it fails to explain the performance improvement of other NPs, even
conductive ones [18]. Furthermore, Sima et al. [10] examined the effect of the conductivity
and permittivity of conductive (Fe3 O4 ), semi-conductive (TiO2 ), and insulating (Al2 O3 )
NPs on transformer oil performances. The ionization models of transformer oil-based NFs
were developed. They concluded that NPs whose conductivity or permittivity mismatch
those of the base liquid increase the saturation charges on their interface, which slows
down the evolution of the streamers, thus enhancing the dielectric strength of NFs.
A. Beroual and H. Duzkaya [19] examined the variation of AC and lightning impulse
(LI) breakdown voltages of natural ester enriched with fullerene (C60 ) nanoparticles for
concentrations ranging from 0.05 to 0.4 g/L. They observed that the AC breakdown voltage
performances of 0.3 and 0.4 g/L C60 nanofluids are increased compared to natural ester.
The increase rate is 5.1% and 7.8%, respectively. A concentration of 0.1 g/L C60 has 8.2%
better performance than natural ester at LI breakdown voltages. Recently, Khelifa et al. [20]
investigated the AC breakdown voltage of a synthetic ester MIDEL 7131-based NFs with
graphene (Gr) and fullerene (C60 ). They found that adding Gr or C60 at different con-
centrations enhances the BDV value, and optimal concentration between 0.3 and 0.4 g/L
gives the best breakdown voltage value. The BDV enhancement is more important with
SE-based NFs with C60 than with Gr for the electrode gaps up to 0.5 mm, with the elec-
trodes being spherical and 12.5 mm in diameter. Beyond this gap, the improvements are
more important with Gr than with C60 . The best improvements for a 2 mm gap are about
12.67% and 16.64%, with C60 (0.4 g/L) and Gr (0.3 g/L), respectively. It was reported from
the literature that most of the published works address the performances of breakdown
voltages of transformer oil-based NFs; the partial discharge (PD) activity on those NFs is
less well-studied in the literature.
Jin et al. [21,22] investigated the PD activity in mineral oil and mineral oil-based NFs
with Fullerene (C60 ) and silica (SiO2 ) NPs at 0.01 wt.% (~0.1 g/L). An enhancement of the
PD inception voltage (PDIV) by 20% with SiO2 and by 10% with C60 was reported. They
attributed this enhancement to the positive effect of hydrophilic silica NPs, which reduce the
moisture content, thus reducing the PD activity. Atiya et al. [23] compared the PD activity
of mineral oil and mineral oil-based Al2 O3 NFs impregned pressboards. They reported that
Al2 O3 NFs impregned pressboard show the highest PDIV. Furthermore, Atiya et al. [24]
investigated the effect of the type of NPs (TiO2 and Al2 O3 ) and the thickness of electrical
double layers (EDL) around the NPs; they were the first to explain such difference in PD
activity by the EDL around NPs [24]. They concluded that the smaller the EDL, the lower
the PD activity. Recently, Khelifa et al. [20] and Koutras et al. [25] reported that the addition
of carbonic (C60 ) and silicon carbide (SiC) NPs enhances the PD resistivity of pure synthetic
ester (MIDEL 7131) and natural ester (FR3), respectively.
This paper is aimed at studying the influence of conducting (Fe3 O4 , 20 nm), semi-
conductive (ZnO, 25 nm), and insulating (ZrO2 , 20–30 nm, SiO2 , 10–20 nm, and Al2 O3 ,
20–30 and 50 nm) nanoparticles (NPs) at various concentrations on the AC dielectric
strength of MIDEL 7131 synthetic ester. First, Section 2 presents a detailed and improved
procedure for preparing NFs in five concentrations ranging from 0.1 g/L to 0.5 g/L,
including high-speed agitation and ultrasonication; the long-term stability checking technic
based on zeta potential analysis is then addressed. After dealing with the preparation
and characterization of NF samples, the following step presents the AC BDV and PD
measurements methodology. Next, section three is devoted to the results of long-term
stability, AC BDV, and PD activity. The conformity of experimental outcomes with normal,
Weibull, and Extreme Values statistic distributions laws are also performed, and the mean
and breakdown voltages at different risk levels were evaluated. Finally, the fourth section
discusses the results and the possible physicochemical processes behind the observed
improvement of AC BDV and PD resistivity.
2. Materials and Methods

2.1. Materials
The used base liquid is the synthetic ester MIDEL 7131 provided by M&I Materials,
Manchester, UK. ZrO2 , SiO2 , and Al2 O3 NPs were supplied by SkySpring Nanomaterials
(SS Nano, Houston, TX, USA), while the ZnO NPs were supplied by PlasmaChem GmbH,
Berlin, Germany. The Fe3 O4 NPs and oleic acid (cis-9-Octadecenoic acid) were supplied by
Sigma-Aldrich (St. Louis, MI, USA). Tables 1 and 2 show the physicochemical properties
of MIDEL 7131 [26] and the characteristic of NPs, respectively. Some properties were not
provided by the suppliers; we indicated those taken from the literature, which are marked
with an asterisk [10]. A high-speed rotor-stator disperser (Misceo, 250 F, Mortagne-sur-
Sèvre, France) and ultrasonic liquid processors device (Sonics, VCX 500, Newtown, CT,
USA) were used to prepare NFs.
Table 1. Physicochemical Properties of Synthetic Ester, MIDEL 7131.
Property MIDEL 7131

Density at 20 ◦C(kg/L) 0.97
Kinematic Viscosity (mm2 /s)
at 40 ◦ C 29
at −20 ◦ C 1440
Pour point (◦ C) −56
Flash point (◦ C) 260
Fire point (◦ C) 316
Water content (ppm) 50
AC BDV “60Hz” (kV) >75
Dielectric constant 3.2
Power Factor at 90 ◦ C <0.008
DC Resistivity at 90 ◦ C (GΩ·m) >20
Table 2. Characteristics of the nanoparticles.
NPs Fe3 O4 ZnO ZrO2 SiO2 Al2 O3 Al2 O3

Size (nm) 20 25 20–30 10–20 20–30 50
Specific surface area
40 19 ± 5 15–35 60–100 120–140 80
(m2 /g)
Density (g/cm3 ) 5.1 * 5.6 4.8–6.0 0.6~1.8 3–3.98 *
Dielectric Constant 80 * 8.5 10–23 3.9 9–10.1 *
Purity (%) 99.5 99.5 99 99.8 99.9 99.9
* The values are taken from literature as they are not provided by the suppliers.
2.2. Samples Preparation

The two-step method was executed for preparing the NFs samples, as depicted
in Figure 1. The base liquid cannot be used in its initial state, and it needs to be purified;
the purification was made using a micro-membrane filter and a vacuum pump to remove
impurities. Oleic acid (used as a surfactant) was then added, and the mixture was stirred
for five minutes using the high-speed rotor-stator mixer at 13,000 rpm. The mass ratio of
oleic acid (OA) to base liquid is 0.75 wt.%. This concentration was based on previous work
within the research team [20]; the evolution of zeta potential versus concentration of OA
has been examined, and the 0.75 wt.% gives the best compromise. Next, the desired weight
of powder NPs was dispersed within the base liquid, and the mixture is agitated for 20 min.
Five concentrations are considered, ranging from 0.1 to 0.5 g/L (0.01 to 0.05 wt.%). Finally,
the samples of NFs are subjected to an ultrasound agitation for two hours to uniformize the
mixture and reach a stable colloid. The Ultrasonic Liquid Processors device (500 W, 20 kHz)
with 25 mm low-intensity solid probe operates in a pulsed mode (i.e., 10 s of operation and
5 s of rest) with an amplitude set of 60%. After every 30 min, the ultrasonic equipment
is rested for 5 min to avoid overheating NF samples and extend the equipment lifetime,
especially the solid probe. Note that the volume of the prepared NFs is 400 mL for each
concentration and type of NPs.
Nanomaterials 2022, 12, 2105
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2105 5 of 25 5 o
Figure 1. The preparation procedure of nanofluids (NFs).
2.3. Stability of Nanofluids

Figure
Figure 1. The
1. The preparation
preparation procedure
procedure of nanofluids
of nanofluids (NFs). (NFs).
The stability was considered to be the most significant issue facing NFs. Un
2.3. Stability
nately, this ofhas
Nanofluids
proven to be a severe impediment to the widespread usage of tho
The stability
uids, especially was considered
for those to be the mostthat
applications significant issue facing NFs. Unfortunately,
The stability was considered to be theneed
most asignificant
considerable
this has proven to be a severe impediment to the widespread usage of those liquids,
issue volume,
facing NFs. as the c
Unfor
power transformers.
nately, thisthose Thus,
has applications
proven to particular
be a severe attention
impediment should
to thebe paid to this
widespread usagestepof for a
those
especially for that need a considerable volume, as the case for power
outcome concerning
uids, especially
transformers. forcolloid
Thus, particular stability.
thoseattention
applications Many
should that techniques
needtoathis
be paid forforchecking
considerable
step volume,
a proper the asstability
outcome w
the case
ported in the literature,
power transformers.
concerning including
colloid stability.Thus,
Manyparticularzeta potential
techniquesattention (ζ-potential)
should
for checking analysis
be paidwere
the stability to this [27]. The
step in
reported ζ-po
for a pro
analysis
theoutcome appears
literature, to be
concerning
including zetathe
colloidmost efficient
stability.
potential Many and
(ζ-potential) less time-consuming
techniques
analysis [27].for
Thechecking the
ζ-potential method
stabilitytowere
analysis che
appears
ported
stability to be
ofinNFsthe most
the [27,28]. efficient
literature, The and
includingless time-consuming
stabilityzeta potential
depends method
on(ζ-potential) to
the ζ-potential check the
analysis stability
value;[27]. of
The ζ-potenp
a schematic
NFsanalysis
[27,28]. appears
The stability depends on the ζ-potential value; a schematic presentation is check
tation is depicted in Figure 2. For the absolute values between 0 and 10 to
to be the most efficient and less time-consuming
depicted in Figure 2. For the absolute values between 0 and 10 mV, the NF is considered
method mV, the
stability
considered of NFs [27,28]. The stability depends on the ζ-potential value; a schematic pres
unstable, andunstable, and action
action is needed is needed
to overcome this. to overcome this.
tation is depicted in Figure 2. For the absolute values between 0 and 10 mV, the NF
considered unstable, and action is needed to overcome this.
Unstable NF Stable NF Highly Stable NF
Unstable NF Stable NF Highly Stable NF
0 10 30 |ζ-potential| (mV)
0 10 30 |ζ-potential| (mV)
Figure 2. Significance
Figure 2. Significance of zeta
of zeta potential
potential values.values.
Figure 2. Significance of zeta potential values.
In contrast, for the absolute values higher than 30 mV, the NFs are considered highly
In contrast, for the absolute values higher than 30 mV, the NFs are considered
stable; between the two ranges, the NFs are stable [28]. The hydrodynamic diameter and
stable; In contrast,
between thefor
twotheranges,
absolutethevalues
NFs higher
are than [28].
stable 30 mV, thehydrodynamic
NFs are considered hig
ζ-potential measurements were performed thrice using a ZetasizerTheNano (ZS) instrument diamet
stable;
ζ-potential between
(Malvern, UK). the
measurements two ranges,
As a supplementwere the NFs
to performed are stable
thrice
zeta potential [28]. The hydrodynamic
using a Zetasizer
measurements, Nano
the Zetasizer diameter
(ZS) instra
Nano
ζ-potential
provides the measurements
electrical were performed thrice usingthea Zetasizer Nano (ZS)ofinstrum
(Malvern, UK). As aconductivity
supplement of to
NFzeta
samples. Therefore,
potential spectral absorbance
measurements, the Zetasizer Nan
(Malvern, UK). As a supplement to zeta potential measurements, the Zetasizer Nano p
vides the electrical conductivity of NF samples. Therefore, the spectralspectral
each sample was checked before performing the measurement. All samples whose
absorbance o
vides theiselectrical
absorbance less than conductivity of NFthe
100 could perform samples. Therefore,
zeta potential the spectral
analysis absorbance
as explained in a of e
sample
previous
sample
was
work checked
was[20]. before
Hence,
checked
performing
only three
before
the
concentrations
performing
measurement. Allsamples
(0.1, 0.2, and 0.3All
the measurement. g/L) samples whose spect
were considered
whose spectral
sorbance
according
sorbanceis
to less
the than 100
absorbance
is less than could
couldperform
perform the
measurement.
100 zeta potential
the zeta potentialanalysis
analysis asas explained
explained in ainp
vious work [20]. Hence, only
onlythree
threeconcentrations (0.1,0.2,
0.2,and
and0.30.3 g/L) were cons
2.4.vious work
Procedure for [20]. Hence,
Breakdown Voltage concentrations (0.1,
Measurement g/L) were conside
according to the absorbance measurement.
according to the absorbance measurement.
The breakdown voltage measurements have been performed in compliance with IEC
60156 standard method using a commercially available BAUR system. The test bench
2.4. Procedure
2.4.
consists Procedurefortank
of an oil Breakdown
for Breakdown Voltage
Voltage
with a capacity Measurement
of 400Measurement
mL, an electrodes system with adjustable gap
distance, The
andbreakdown
a high voltagevoltage measurements
generator
The breakdown voltage measurements that can have
reach 100been
have kV RMS
been performed
(50 Hz). in
performed compliance
According
in to with
compliance wI
IEC60156
60156standard
[29], the BDV test
method is performed in
usingaacommercially a sphere-sphere
commercially available electrode configuration of
60156 standard method using availableBAUR
BAURsystem.system. The testtest
The bench c
benc
12.5sists
mm of diameter,
an oil with awith
tank spacing
a of 2.5 mm.
capacity The voltage iselectrodes
applied continuously with an
sists of anofoil
increment tankuntil
2 kV/s with a capacity
breakdown of 400 mL, an electrodes system with adjustabg
of
occurs.
400 mL, an system with adjustable
distance, and a high voltage generator that can reach 100 kV RMS (50 Hz). According
distance,
Fe O4andandaAl high voltage
O3 NFs showgenerator that canstrength,
superior dielectric reach 100 kV RMS
exceeding the (50 Hz). Accord
oil tester
IEC360156 [29],2 the BDV test is performed in a sphere-sphere electrode configuration
limitation
IEC 60156(100[29],kV);
theforBDV
that test
reason, a reduced electrode
is performed gap to 2 mm iselectrode
in a sphere-sphere consideredconfigura
to
12.5 mm
compare the diameter, with
breakdown voltagea spacing
of the ofNPs.
six 2.5 mm.
In The voltage
addition, the BDVis test
applied
is continuously
carried out for with
12.5increment
mm diameter,of 2 with
kV/s a spacing
until breakdown of 2.5 mm. The voltage is applied continuously w
occurs.
NFs in which the breakdown occurs for an electrodes gap of 2.5 mm (i.e., ZnO, ZrO2 , and
incrementFe3of
O4 2and
kV/sAl2until
O3 NFsbreakdown occurs.
show superior dielectric strength, exceeding the oil tester li
Fe3O(100
tation 4 and Al2for
kV); O3 that
NFsreason,
show superior
a reduceddielectric strength,
electrode gap exceeding
to 2 mm the oil
is considered teste
to comp
tation (100 kV); for that reason, a reduced electrode gap to 2 mm is considered
the breakdown voltage of the six NPs. In addition, the BDV test is carried out for NFs to co
the which
breakdown voltage of
the breakdown the six
occurs for NPs. In addition,
an electrodes gap ofthe2.5BDV test is
mm (i.e., carried
ZnO, ZrO2out
, andfor
SiO

and 2.5 mm electrode gaps to the extreme value (EV), Weibull, and normal distr
were analyzed using Anderson–Darling statistics. The EV distribution is rarely
analyze AC-BDV data [13], unlike the widely used Weibull and normal distribu
SiO2 ). Three series of six measurements have been performed, giving 18 points considered
nally, the
sufficient for voltages corresponding
the statistical analysis [13,16].to 1%,the
Next, 10%, and 50%
conformity risk
of AC levels
BDV data were determin
for 2 mm
the2.5
and normal and EVgaps
mm electrode distributions.
to the extreme value (EV), Weibull, and normal distributions
were analyzed using Anderson–Darling statistics. The EV distribution is rarely used to
analyze AC-BDV data [13], unlike the widely used Weibull and normal distributions.
2.5. Partial Discharges Measurement under AC 50 Hz Stress
Finally, the voltages corresponding to 1%, 10%, and 50% risk levels were determined using
The and
the normal partial discharges (PDs) activity in both SE and the three SE-based NFs
EV distributions.
the best improvement in AC BDV tests are conducted in compliance with IEC 6027
2.5. Partial Discharges Measurement under AC 50 Hz Stress
ard method; in this case, Fe3O4 (20 nm) and Al2O3 (50 nm) at optimal concentratio
The partial discharges (PDs) activity in both SE and the three SE-based NFs that
and Al2O3 (20–30 nm) at optimal concentration 0.3 g/L. An industrial Omicron PD
give the best improvement in AC BDV tests are conducted in compliance with IEC 60270
detection
standard was used
method; in thisfor this
case, Fe3purpose.
O4 (20 nm)Theand PDs
Al2 O3test
(50 is
nm)performed in a needle-plane e
at optimal concentration
configuration;
0.4 the gap
g/L and Al2 O3 (20–30 nm)between
at optimalthe two electrodes
concentration 0.3 g/L.isAn5industrial
mm. TheOmicron
tip radius
PDs of cur
system
10 μm, detection
while the wasplane
used for this purpose.
electrode has aThe
35PDs
mmtest is performed
diameter. Theinapplied
a needle-plane
voltage is var
electrode configuration; the gap between the two electrodes is 5 mm. The tip radius of
its RMS value follows the profile depicted in Figure 3; the voltage rises and fal
curvature is 10 µm, while the plane electrode has a 35 mm diameter. The applied voltage is
speedand
varied, of 1itskV/s,
RMS 13 kVfollows
value as thethemaximum value in
profile depicted onFigure
the plateau, maintained
3; the voltage rises and for 32 s
of rest
falls withisa respected between
speed of 1 kV/s, 13 kVtwo successive
as the tests on
maximum value from
the the same
plateau, series. This
maintained for voltag
32 s, and 5 s of rest is respected between two successive tests from the same
is repeated five times for each sample, which underwent five PDs tests for each li series. This
voltage profile isvalues
the collected repeatedpresent
five times
theforaverage
each sample, which
of five underwent five PDs tests for
measurements.
each liquid. So, the collected values present the average of five measurements.
15
10
0
0 50 100 150 200 250 300
Time (s)
Figure
Figure 3. Voltage
3. Voltage profile
profile (RMSapplied
(RMS value) value)toapplied
samplesto samples
during partialduring partial
discharge test. discharge test.
For the comparison and quantification of PD activity, we are interested in the PD

For the comparison and quantification of PD activity, we are interested in
inception voltage (PDIV), PD extinction voltage (PDEV) during raise and falling times,
inception and
respectively, voltage
average(PDIV),
charge (QPD extinction voltage (PDEV) during raise and fallin
avg ), peak charge (Qpeak ), and number of PDs (NPDs/s)
respectively, and average charge (QItavgis),about
during the voltage plateau (at 13 kV RMS). peakthecharge
average(Qcharge
peak), and number
and the numberof PDs (
of PDs perthe
during second (NPD/s)
voltage during
plateau (atthe
13 32kVs,RMS).
while QItpeak is the highest
is about charge charge
the average recordedand the
in the same interval. In addition, the phase-resolved PDs pattern is also compared and
of PDs per second (NPD/s) during the 32 s, while Qpeak is the highest charge rec
plotted for the four liquids.
the same interval. In addition, the phase-resolved PDs pattern is also compared a
3.ted
Results
for the four liquids.
As mentioned above, the hydrodynamic diameter and zeta potential measurements
3. Results
are performed on the NFs samples. However, hydrodynamic diameter analysis does not
3.1.an
give Stability of Nanofluids
affirmative indication of the stability of NFs. For that reason, one concentration
is considered in this
As mentioned analysis
above,for the
thesix NFs to show thediameter
hydrodynamic dispersionand
behavior
zetaand look at
potential
measu
are performed on the NFs samples. However, hydrodynamic diameter analysis
give an affirmative indication of the stability of NFs. For that reason, one concent
considered in this analysis for the six NFs to show the dispersion behavior and lo
agglomerations/clusters present in the liquid. Figure 4 shows the size distribution

the agglomerations/clusters present in the liquid. Figure 4 shows the size distributions of
7 of 25
different SE-based NFs for a specified concentration (0.1 g/L). For all NF samples, it was
noticed that maximum intensities reveal sizes higher than the declared ones by the sup-
plier (Figure 4b). Since the observed/measured diameter using Dynamic Light Scattering
does not
(DLS) exclusively
does consider
not exclusively the particle
consider size, unlike
the particle size,to NPs size
unlike measurement
to NPs by micros-
size measurement by
copy technics
microscopy (SEM and
technics (SEM TEM); oleic acid
and TEM); oleicenvelopes the NP,
acid envelopes thepossibly leading
NP, possibly to an over-
leading to an
estimation (an increase
overestimation of theofsize),
(an increase thus thus
the size), to larger sizes sizes
to larger than than
expected. [30]. Furthermore,
expected. [30]. Further-
from what the suppliers claim, Fe
more, from what the suppliers claim, Fe3 O4 (20 nm), ZnO (25 nm), and Al2nm)
3 O4 (20 nm), ZnO (25 nm), and Al 2O 3 (50 NPs
O3 (50 should
nm) NPs
present a size distribution with a high peak around a specific diameter
should present a size distribution with a high peak around a specific diameter (theoretically(theoretically
around the declared
around the declared sizes),
sizes), and
and ZrO
ZrO22 (20–30
(20–30 nm),
nm), SiO
SiO22 NPs
NPs (10–20
(10–20 nm),
nm), and
and AlAl22O
O33 (20–30
(20–30
nm) should be
nm) should be much
much larger
larger (large
(large variation
variation sizes
sizes with
with aa smaller
smaller peak),
peak), while
while only
only ZrO
ZrO22
(20–30 nm) and Al22O33 (20–30
(20–30 nm)
nm) NPsNPs fit
fit this
this description.
description.
(a) (b)
Figure 4. Nanoparticle size distribution (a,b).
Figure 4. Nanoparticle size distribution (a,b).
For
For the
the zeta
zeta potential
potential analysis,
analysis, thethe measurement
measurement is is performed
performed for for the
the three
three concen-
concen-
trations in which the absorbance
absorbance values
values areare below
below 100,
100, which
which indicates
indicatesthethetest
testfeasibility.
feasibility.
Table 33 gives
Table givesaasummary
summaryofofζ-potential
ζ-potentialand andelectrical
electrical conductivity
conductivity results
results forfor three
three con-
concen-
centrations taken one week after the preparation. According to the
trations taken one week after the preparation. According to the results, SiO2 (10–20 nm) results, SiO 2 (10–20
nm)
NF isNF is highly
highly stable,
stable, while
while thethe other
other NFsNFsareare stable.We
stable. Wecould
couldspeculate
speculatethisthisto
to the
the size
difference (contact surface); SiO22 (10–20(10–20 nm)
nm) is is the smaller NPs, which should provide a
more significant contact surface NPs/liquid
NPs/liquid than than the
the other
other NPs.
NPs.
Note that after three weeks, we did not observe sedimentation. However, if the zeta
potential
potential indicates
indicatesthat
thatNFs
NFsremain
remainstable,
stable,this
thiscannot
cannot bebe
a guarantee
a guarantee of of
stability forfor
stability several
sev-
years and the
eral years andlifetime of the
the lifetime oftransformer.
the transformer.
Moreover, the electrical conductivity of ZrO2 (20–30 nm), SiO2 (10–20 nm), and Al2 O3
Table 3.and
(20–30 Zeta50potential
nm) NFs and electricalwith
decrease conductivity of nanofluids
concentration, whilesamples.
it increases with Fe3 O4 (20 nm)
and ZnO (25 nm) NFs. This is because ZrO2 , SiO2 , and Al2 O3 are insulation NPs, while
Zeta Potential Elec. Conductivity
ZnO is semi-conductive NPs, NFsand Fe3 O4 is conductive NPs. Those fundamental differences
may justify the observed differences. (mV) (mS/cm) × 10–3
SE/Fe3O4 (20 nm) –22.4 2.16
3.2. AC Breakdown VoltageSE/ZnOTest(25
for nm)
2 mm Electrodes Gap +22.9 0.94
SE/ZrO (20–30 nm) –24.4
As explained in the previous section, the breakdown does not occur at a 2.5 mm
2 2.09
(0.1 g/L)
electrode gap with SE/SiO 2 (10–20
Fe3 O4 (20 nm) Al2 O3 (20–30
nm) and –36.2
and 50 nm) NFs; the 1.73 AC BDV with a
2 mm electrode gap distance
SE/Al is also
2O3 (20–30 nm)considered to compare the six NPs under
+15.9 1.24 the same
experimental conditions,SE/Alwhich
2O3 (50is the purpose of+24.9
nm) this subsection. Figure1.37 5a–f shows the
mean and max/minSE/Fe AC BDV for
3O4 (20 nm)Synthetic Ester and Fe
–23.6 3 4 O (20 nm), ZnO (25 nm), ZrO2
2.31
(20–30 nm), SiO2 (10–20 nm), and
SE/ZnO (25 nm) Al O
2 3 (20–30 and 50
+19.7 nm) NFs at different concentrations,
1.26
respectively. Whatever the type and concentration of the used NPs, the enhancement of the
SE/ZrO2 (20–30 nm) –21.8 1.89
(0.2
BDVg/L)
in NFs was remarkable compared to the pure SE. In addition, adding NPs reduces the
SE/SiO2 (10–20 nm) –33.7 1.57
SE/Al2O3 (20–30nm) +20.4 0.85
SE/Al2O3 (50 nm) +29.0 1.06
(0.3 g/L) SE/Fe3O4 (20 nm) –17.9 2.78
standard deviation of AC BDV which mainly increases the slope in the statistical analysis,
thence enhancing the BDV at low-risk levels. Furthermore, the type and concentrations
of NPs play a significant role in increment percentage. Synthetic ester-based ZnO (25 nm,
ZrO2 (20–30 nm), and SiO2 (10–20 nm) NPs manifested the best improvements of around
20% compared to pure SE, while the best improvements with Fe3 O4 (20 nm) and Al2 O3
(20–30 and 50 nm) NFs NPs were between 37% and 44% concerning pure SE. Those im-
provements were compared and plotted, as depicted in Figure 6. It was noted that all NFs
samples reveal an optimal concentration of around 0.3 and 0.4 g/L.
Table 3. Zeta potential and electrical conductivity of nanofluids samples.
Elec. Conductivity
NFs Zeta Potential (mV)
(mS/cm) × 10−3
SE/Fe3 O4 (20 nm) −22.4 2.16
SE/ZnO (25 nm) +22.9 0.94
SE/ZrO2 (20–30 nm) −24.4 2.09
(0.1 g/L) SE/SiO2 (10–20 nm) −36.2 1.73
SE/Al2 O3 (20–30 nm) +15.9 1.24
SE/Al2 O3 (50 nm) +24.9 1.37
SE/Fe3 O4 (20 nm) −23.6 2.31
SE/ZnO (25 nm) +19.7 1.26
SE/ZrO2 (20–30 nm) −21.8 1.89
(0.2 g/L) SE/SiO2 (10–20 nm) −33.7 1.57
SE/Al2 O3 (20–30nm) +20.4 0.85
SE/Al2 O3 (50 nm) +29.0 1.06
SE/Fe3 O4 (20 nm) −17.9 2.78
SE/ZnO (25 nm) +17.0 1.41
SE/ZrO2 (20–30 nm) - -
(0.3 g/L) SE/SiO2 (10–20 nm) −31.9 1.02
SE/Al2 O3 (20–30 nm) - -
SE/Al2 O3 (50 nm) +21.0 0.67
Note that with the optimal concentration of SiO2 (10–20 nm) and Al2 O3 (20–30 nm)
NPs that is 0.3 g/L, the BDV is improved by 20.30% and 44.12%, respectively, as shown
in Figure 5d,e. Up to 0.3 g/L, a slight lowering for the same Al2 O3 NPs of 50 nm is remarked
compared to the smaller Al2 O3 of 20 nm NPs; a reversed tendency is observed beyond
0.4 g/L. With 0.4 g/L Al2 O3 (50 nm), the enhancement is 42.13% compared to pure SE
(Figure 5f). Khaled and Beroual have also carried out conceptually similar work [15,16]
in which Al2 O3 (13 and 50 nm) NPs dispersed within mineral oil and synthetic ester,
where they showed a similar tendency: the smallest particles provide a lower optimal
concentration. With Fe3 O4 (20 nm), ZnO (25 nm), and ZrO2 (20–30 nm) NPs, the best
enhancements are about 37.70%, 19.38%, and 21.37%, respectively, for a concentration of
0.4 g/L, as shown in Figure 5a–c. Fe3 O4 (20 nm) and Al2 O3 (20–30 nm and 50 nm) NFs
show the best performances according to AC BDV; their best improvements are greater
than 35% for all cases.
3.3. AC Breakdown Voltage Test for 2.5 mm Electrode Gap (IEC 60156)
Following the IEC 60156 standard (2.5 mm electrode gap), among the six tested NPs,
the breakdown occurs only with ZnO (25 nm), ZrO2 (20–30 nm), and SiO2 (10–20 nm) NFs.
Therefore, only the three NPs will be addressed in the following section. Figures 7–9 give
the mean and max/min AC BDV for synthetic ester-based ZnO (25 nm), ZrO2 (20–30 nm),
and SiO2 (10–20 nm) NFs at different concentrations, respectively. It was noted that the
best enhancements of SE-based ZnO (25 nm) and ZrO2 (20–30 nm) NFs, are about 14.28%
and 11.13%, respectively, for a concentration of 0.4 g/L, as shown in Figures 7 and 8, while
for SE-based SiO2 (10–20 nm) NFs, the improvement reaches the highest BDV value for a
concentration of 0.3 g/L (Figure 9); this presents a 12.83% of improvement against pure SE.
the standard deviation of AC BDV which mainly increases the slope in the statistical anal-
ysis, thence enhancing the BDV at low-risk levels. Furthermore, the type and concentra-
tions of NPs play a significant role in increment percentage. Synthetic ester-based ZnO (25
nm, ZrO2 (20–30 nm), and SiO2 (10–20 nm) NPs manifested the best improvements of
Nanomaterials 2022, 12, 2105 around 20% compared to pure SE, while the best improvements with Fe3O4 (209 of nm)
25 and
Al2O3 (20–30 and 50 nm) NFs NPs were between 37% and 44% concerning pure SE. Those
improvements were compared and plotted, as depicted in Figure 6. It was noted that all
NFsFinally,
samplesthe improvements were concentration
reveal an optimal compared and plotted for each
of around concentration,
0.3 and 0.4 g/L. as depicted
in Figure 10.
Mean AC BDV, SE/Fe3O4 Max/Min values Mean AC BDV, SE/ZnO Max/Min values
100 100
80 80
60 60
40 40
20 20
0 0
SE 0.1 0.2 0.3 0.4 0.5 SE 0.1 0.2 0.3 0.4 0.5 9 of 25
Concentration (g/L) Concentration (g/L)
(a) (b)
Mean AC BDV, SE/ZrO2 Max/Min values Mean AC BDV, SE/SiO2 Max/Min values
100 100
80 80
60 60
40 40
20 20
0 0
SE 0.1 0.2 0.3 0.4 0.5 SE 0.1 0.2 0.3 0.4 0.5
(c) (d)
Mean AC BDV, SE/Al2O3 (20–30nm) Max/Min values Mean AC BDV, SE/Al2O3 (50nm) Max/Min values
100 100
80 80
60 60
40 40
20 20
0 0
SE 0.1 0.2 0.3 0.4 0.5 SE 0.1 0.2 0.3 0.4 0.5
(e) (f)
Figure 5. 5.
Figure Mean
Meanbreakdown voltagesofofsynthetic
breakdown voltages synthetic ester
ester andand synthetic
synthetic ester-based
ester-based nanofluid
nanofluid at differ-
at different
entconcentrations
concentrations of of nanoparticles:
nanoparticles: (a) Fe Fe3O4 (20 nm), (b) ZnO (25 nm), (c) ZrO2 (20–30 nm), (d) SiO2
(a) O
3 4 (20 nm), (b) ZnO (25 nm), (c) ZrO2 (20–30 nm), (d) SiO2
(10–20 nm), (e) Al 2O3 (20–30 nm), (f) Al2O3 (50 nm).
(10–20 nm), (e) Al O (20–30 nm), (f) Al O (50 nm).
2 3 2 3
60
SE/Fe O
3 4
SE/ZnO
50 SE/ZrO
2
SE/SiO
2
SE/Al 2O 3 (20–30 nm)
40 SE/Al 2O 3 (50 nm)
30
SE 0.1 0.2 0.3 0.4 0.5 SE 0.1 0.2 0.3 0.4 0.5
(e) (f)
With Fe
Figure 3O4 (20 nm), ZnO (25 nm), and ZrO2 (20–30 nm) NPs, the best enhancem
5.3Mean breakdown voltages of synthetic ester and synthetic ester-based nanofluid
With
about Fe O 4 (20 nm), ZnO (25 nm), and ZrO2 (20–30 nm) NPs, the best enhancem
37.70%, 19.38%, and 21.37%,
Nanomaterials 2022, 12, 2105 ent concentrations of nanoparticles: (a) Ferespectively, for a concentration10of
3O4 (20 nm), (b) ZnO (25 nm), (c) ZrO 2of
0.4
25 g/L,
(20–30 nm)a
about 37.70%,
in Figure 19.38%, and 21.37%, respectively, for a concentration of 0.4 g/L, a
(10–20 nm),5a–c.
(e) AlFe
2O33O 4 (20 nm)
(20–30 nm), and
(f) AlAl
2O23O3 (20–30
(50 nm). nm and 50 nm) NFs show the bes
in Figure 5a–c. Fe 3O4 (20 nm) and Al2O3 (20–30 nm and 50 nm) NFs show the bes
mances according to AC BDV; their best improvements are greater than 35% for
mances according to AC BDV; their best improvements are greater than 35% for a
60
SE/Fe O
3.3. AC Breakdown
SE/ZnO
3 4 Voltage Test for 2.5 mm Electrode Gap (IEC 60156)
3.3.50 AC Breakdown
SE/ZrO Voltage Test for 2.5 mm Electrode Gap (IEC 60156)
Following
SE/SiO
2
the IEC 60156 standard (2.5 mm electrode gap), among the six tes
the Following
breakdown occurs
SE/Al O
2
2
the
(20–30
3
nm)
IEC only
60156with
standard
ZnO (25 (2.5nm),
mmZrOelectrode gap), among the six test
2 (20–30 nm), and SiO2 (10–20 n
40
the breakdown
Therefore, onlyoccurs
SE/Al O (50 nm)
2 3
the threeonlyNPs
with ZnO
will be (25 nm), ZrO
addressed (20–30
in2 the nm), and
following SiO2 (10–20
section. Figures n
Therefore,
the only the three NPs will be addressed in the following section. Figures
30 mean and max/min AC BDV for synthetic ester-based ZnO (25 nm), ZrO2 (20
the
andmean SiO2 and (10–20 max/minnm) NFs ACat BDV for synthetic
different ester-based
concentrations, ZnO (25 nm),
respectively. ZrOnoted
It was 2 (20–
and20 SiO2 (10–20 nm) NFs at different concentrations, respectively. It was noted
best enhancements of SE-based ZnO (25 nm) and ZrO2 (20–30 nm) NFs, are abou
best
and enhancements
11.13%, respectively, of SE-based ZnO (25 nm) and
for a concentration of 0.4ZrO
g/L,2 (20–30 nm) NFs, are abou
as shown in Figures 7 and
10
and 11.13%, respectively, for a concentration
for SE-based SiO2 (10–20 nm) NFs, the improvement reaches of 0.4 g/L, as shown theinhighest
FiguresBDV7 andva
for SE-based
concentration
0
SiO of 2 (10–20 nm) NFs, the improvement reaches the highest BDV va
0.3 g/L0.3(Figure0.49); this presents a 12.83% of improvement aga
0.1 0.2 0.5
concentration of
SE. Finally, the improvements 0.3 g/L (Figure 9); this presents a 12.83% of improvement again
Concentration (g/L)were compared and plotted for each concentratio
SE.
pictedFinally,
in Figurethe improvements were compared and plotted for each concentration
10. the improvements
Figure
Figure 6. 6. Comparison
Comparison
picted in Figure 10. between
between the improvements of breakdown
of breakdown voltages
voltages of different of different
nanofluids for nano
different
different concentrations.
concentrations.
Mean AC BDV, SE/ZnO Max/Min values
100
100
Note thatMean
withAC BDV,
theSE/ZnO
optimalMax/Min values
concentration of SiO2 (10–20 nm) and Al2O3 (20
NPs that is 0.3 g/L, the BDV is improved by 20.30% and 44.12%, respectively, as s
80
Figure
80 5d,e. Up to 0.3 g/L, a slight lowering for the same Al2O3 NPs of 50 nm is re
compared
60
to the smaller Al2O3 of 20 nm NPs; a reversed tendency is observed bey
g/L.60With 0.4 g/L Al2O3 (50 nm), the enhancement is 42.13% compared to pure SE
5f). Khaled
40 and Beroual have also carried out conceptually similar work [15,16] i
40
Al2O3 (13 and 50 nm) NPs dispersed within mineral oil and synthetic ester, wh
showed
20 a similar tendency: the smallest particles provide a lower optimal concen
20
0
0 SE 0.1 0.2 0.3 0.4 0.5
SE 0.1 Concentration
0.2 0.3 (g/L) 0.4 0.5
Concentration (g/L)
Figure 7. Mean breakdown voltages of synthetic ester and synthetic ester-based ZnO
Figure
Figure 7. 7.Mean
nanofluids Mean breakdown
at breakdown
different voltages
voltages of synthetic
of synthetic
concentrations. ester and ester and
synthetic syntheticZnO
ZnO
ester-based ester-based
(25 nm)
nanofluids
nanofluids at different concentrations.
at different concentrations.
Mean AC BDV, SE/ZrO 2 Max/Min values

100 Mean AC BDV, SE/ZrO 2 Max/Min values
100
80
80
60
60
40
40
20
20
0
0 SE 0.1 0.2 0.3 0.4 0.5
0.2 0.3(g/L) 0.4 0.5
Concentration (g/L)
Figure
Figure 8. Mean
8. Mean breakdown
breakdown voltagesvoltages of synthetic
of synthetic ester and
ester and synthetic synthetic
ester-based ZrOester-based
2 (20–30 nm) ZrO2 (2
Figure 8.
nanofluids Mean
at breakdown
different voltages
concentrations.
nanofluids at different concentrations. of synthetic ester and synthetic ester-based ZrO2 (20
nanofluids at different concentrations.
Nanomaterials 2022,
Nanomaterials 12,12,
2022, 2105
2105 11 of 25
Mean AC BDV, SE/SiO2 Max/Min values

100 Mean AC BDV, SE/SiO2 Max/Min values
100
80
80
60
60
40
40
20
20
0
SE 0.1 0.2 0.3 0.4 0.5
0
0.2 0.3(g/L) 0.4 0.5
Concentration (g/L)
Figure 9. Mean breakdown voltages of synthetic ester and synthetic ester-based SiO2 (1
Figure
Figure 9. 9.
nanofluids Mean
Mean breakdown
atbreakdown
different voltages
voltages of synthetic
of synthetic
concentrations. ester and
ester and synthetic synthetic
ester-based(10ester-based
SiO2 (10–20 nm) SiO2
nanofluids
nanofluids at different
at different concentrations.
concentrations.
18
SE/ZnO SE/ZrO 2 SE/SiO 2
18
16 SE/ZnO SE/ZrO 2 SE/SiO 2
16
14
14
12
12
10
10
8
8
6
6
4
4
2
2
0
0.1 0.2 0.3 0.4 0.5
0
0.1 0.2 Concentration
0.3 (g/L)0.4 0.5
Concentration (g/L)
Figure
Figure Comparison
10.10. between
Comparison the improvements
between of breakdownof
the improvements voltages of different
breakdown nanofluids
voltages for
of different n
Figure
different 10. Comparison
concentrations.
for different between the improvements of breakdown voltages of different na
concentrations.
for different concentrations.
3.4. Statistical Analysis of AC Breakdown Voltage Data
3.4.Extreme
Statistical
valueAnalysis of AC and
(EV), normal, Breakdown Voltage Dataare used to analyze and test
Weibull distributions
3.4. Statistical
the conformity Analysis of AC Breakdown Voltage Data
Extremeofvalue
breakdown (EV),voltage
normal, outcomes.
and WeibullContrary to the popular are
distributions statistical
used lawsto analyze
(i.e., Weibull
Extreme and value
normal)(EV),[16,20,25,31],
normal, EVandhas been
Weibullrarelydistributions
considered to adjust are the experi-
used to analyze
the conformity of breakdown voltage outcomes. Contrary to the popular statist
mental AC BDV outcomes [13]. EV distribution combines Gumbel, Frechet, and Weibull
the conformity
(i.e., Weibull of breakdown voltage outcomes. Contrary to the popular statisti
distribution [13];and
hence normal)
probability[16,20,25,31],
fit curves of the EVexperimental
has been rarely resultsconsidered
are plotted usingto adjust th
(i.e.,
imental
EV Weibull
and normalAC BDVand normal)
outcomes
distribution. [16,20,25,31],
Those[13].
latterEV EV
aredistributionhas been rarely
combines
used then to estimate considered
Gumbel,
the voltage to adjust
Frechet,
at specific th
and
imental
risk levels.AC
distribution BDV
[13]; outcomes
Therefore, [13].BDV
the mostprobability
hence crucial EVlevels
distribution
fit shouldofbethe
curves combines
estimated atGumbel,
experimental 1%, 10%, Frechet,
and
results 50% and
are plott
distribution
risk levels.
EV and normal [13];distribution.
Before hence probability
estimating those
Thosefit
voltages, a curvesareof
goodness-of-fit
latter the then
used experimental
test should be results
performed
to estimate are plotte
to
the voltage at
check
EV if
and the data
normal came from
distribution.a population
Those with
lattera specific
are used distribution.
then to If the
estimatedistribution
the voltage at
risk the
obeys levels. Therefore,
experimental data,the most crucial
the voltages could beBDV levels
estimated, andshould be thence
the results estimated
presentat 1%, 1
risk
50% levels.
risk Therefore,
levels.
a good estimation. Before the most
estimating crucialthoseBDV levels
voltages, should
a be estimated
goodness-of-fit testatshould
1%, 1
50%
formed risktolevels.
check
Nevertheless, Before
the the estimating
ifconformity
data of came those avoltages,
from
the experimental population
data wasa goodness-of-fit
with a specific
investigated usingtesttheshould
distributio
formed to check
Anderson–Darling
distribution obeys if the
test. the
The data came from
Anderson–Darling
experimental data,a(AD)population
the statistic iswith
voltages abespecific
a goodness-of-fit
could estimated,distributio
test and th
mainly used
distribution to decide
obeys whether a sample
the experimental of size n is drawn from a specified distribution,
thence present a good estimation. data, the voltages could be estimated, and the
most commonly whether the sample data is drawn from a normal distribution. This test
thence present a good
Nevertheless, theestimation.
conformity of the experimental data wasgoodness-
investigated u
has been successfully extended to the other distributions [32]. Anderson–Darling
of-fit Nevertheless,
Anderson–Darling
is performed to check the
test.conformity
The
if the of the
Anderson–Darling
experimental experimental
data comes from (AD) data
EV,statistic was
normal, and investigated
is Weibull
a goodness-o u
Anderson–Darling test. The Anderson–Darling
mainly used to decide whether a sample of size n is drawn from a specified dist (AD) statistic is a goodness-o
mainly used to decide
most commonly whether whether a sample
the sample dataofissizedrawnn is drawn
from a from normal a specified
distribution.distr
most
has been commonly whether
successfully the sample
extended to the data
other is drawn from a [32].
distributions normal distribution. T
Anderson–Darlin
has been successfully
ness-of-fit is performed extended
to check to ifthetheother distributions
experimental data[32].
comes Anderson–Darlin
from EV, norm
distribution. The conformity is then decided according to the p-value, depending on the
AD value [32,33]. Based on the statistics, if the p-value (probability value) is higher than
the significance level, alpha (α), there is enough evidence to accept the hypothesis that the
data come from a specific distribution. The p-values of 0.05 were considered statistically
significant [13,16,33], and from the AD test, the p-value for the EV, normal, and Weibull
distributions were calculated and compared to the significance level.
3.4.1. Statistical Analysis of AC Breakdown Voltage Outcomes for 2 mm Electrodes Gap

The Anderson–Darling goodness-of-fit was performed on experimental data of the
six NFs at different concentrations for the 2 mm electrode gap in which the breakdown
occurs at this gap distance; the results are shown in Table 4. It was noticed that the p-value
is higher than the significance level for most cases, and therefore, the experimental data
obey the three distributions for those higher than the significance level. According to these
results, the experimental data of AC BDV for the 2 mm electrode gap fit better to the normal
distribution than the EV and Weibull distributions. In addition, the EV and Weibull gave
quite the same p-values since the Weibull is a particular case of EV [13].
Table 4. Hypothesis test of conformity of breakdown voltage outcomes of various nanofluids to EV,
normal, and Weibull distributions considering p-value calculation for the 2 mm electrode gaps.
EV Normal Weibull
Concentration p-Value Decision p-Value Decision p-Value Decision
Pure SE 0.2621 Accepted 0.1175 Accepted 0.2020 Accepted
SE-based NFs with Fe3 O4 (20 nm)
(0.1 g/L) 0.3170 Accepted 0.2484 Accepted 0.4167 Accepted
(0.4 g/L) 0.0262 Not-Accepted 0.2699 Accepted 0.0387 Not-Accepted
SE-based NFs with ZnO (25 nm)
(0.1 g/L) 0.0250 Not-Accepted 0.5068 Accepted 0.0564 Accepted
(0.5 g/L) 0.0410 Not-Accepted 0.0050 Not-Accepted 0.0247 Not-Accepted
SE-based NFs with ZrO2 (20–30 nm)
(0.1 g/L) 0.0394 Not-Accepted 0.3584 Accepted 0.0889 Accepted
SE-based NFs with SiO2 (25 nm)
SE-based NFs with Al2 O3 (20–30 nm)
(0.4 g/L) 0.3330 Accepted 0.0459 Not-Accepted 0.3060 Accepted
SE-based NFs with Al2 O3 (50 nm)
(0.5 g/L) 0.4755 Accepted 0.0203 Not-Accepted 0.3848 Accepted
Figures 11–16 show the normal and EV probability density plot of Fe3 O4 (20 nm), ZnO
(20 nm), ZrO2 (20–30 nm), SiO2 (10–20 nm), Al2 O3 (20–30 nm), and Al2 O3 (50 nm) NFs
(0.2 g/L) 0.0009versusNot-Accepted
AC BDV for different 0.0056 Not-Accepted
concentrations; they show how 0.0012the breakdown Not-Accepted
data fit each
(0.3 g/L) 0.7286 case’s corresponding
Accepted normal and EV probability
0.3314 Accepted lines. From0.6836
those plots, theAcceptedBDV at risk
(0.4 g/L) 0.5240levels (1%, Accepted
10%, and 50%) are 0.2928 Accepted
evaluated from normal and EV 0.5125
distribution fit Accepted
curves and
(0.5 g/L) 0.4755 presented in Table
Accepted 5a,b. The BDV
0.0203 at 1% and 10%
Not-Accepted risk levels (U
0.3848
1% and U ) are
10% Accepted essential
information about the reliability of the HV apparatuses since they represent their voltage
limitFigures
for safe/continuous
11–16 show the operation
normaland andthe
EV lowest possible
probability AC BDV,
density while
plot of Fe33Othe BDV at 50%
44 (20 nm), ZnO
(U50%
(20 ) isZrO
nm), an estimation
2
2 (20–30 of
nm), the
SiO expected
2
2 (10–20 mean
nm), Al BDV
2 O
2 33 [25].
(20–30 nm), and Al 2
2 3O 3 (50 nm) NFs ver-
sus ACIt resorts
BDV for from the results
different in Table 5a,bthey
concentrations; thatshow
the addition
how theofbreakdown
the Fe3 O4 (20 nm),
data ZnO
fit each
(25 nm), ZrO 2
case’s corresponding(20–30 nm), SiO
normal and (10–20 nm),
2 EV probability Al O (20–30
2 lines.
3 nm), and Al
From those plots,2 theO 3 BDV at NPs
(50 nm) risk
could not only enhance the mean AC BDV (from 50% risk level)
levels (1%, 10%, and 50%) are evaluated from normal and EV distribution fit curvesbut also improve theand
AC
BDV at 1% and 10% risk levels. Mainly, the addition
presented in Table 5a,b. The BDV at 1% and 10% risk levels (U1% of these NPs strongly
1% and U10% affects
10%) are essential the
U1% rather than
information about U10%
the and U50% , of
reliability exceeding 75% of improvement
the HV apparatuses since theywith Fe3 O4their
represent (20 nm) and
voltage
Al2 O3 (20–30 and 50 nm) compared to pure SE. Still, Fe3 O4 (20 nm) and Al2 O3 (20–30 and
limit for safe/continuous operation and the lowest possible AC BDV, while the BDV at
50 nm) 50%
give the best U10% and U50% compared to ZnO (25 nm), ZrO2 (20–30 nm), and SiO2
50% (U50% ) is an estimation of the expected mean BDV [25].
(10–20 nm) NFs.
Data (SE)
Data (SE) Data (SE)
(SE)
Data
Fit (SE)
Fit (SE)
Fit (SE)
Fit (SE)
Data (Fe
Data (Fe 3O
O 4,, 0.1
0.1 g/L)
g/L)
3 4 0.9999 Data (Fe
Data (Fe 3O
O4,, 0.1
0.1 g/L)
g/L)
0.9999 Fit (Fe
(Fe 3O
O ,, 0.1
0.1 g/L)
g/L) 0.9999 3 4
0.9999 Fit 3 44 0.99
0.99 Fit (Fe
Fit (Fe3O
O ,, 0.1
0.1 g/L)
g/L)
0.999
0.999 Data (Fe
(Fe 3O
O ,, 0.2
0.2 g/L)
g/L) 3 44
Data 3 44 0.9
0.9 Data (Fe
Data (Fe 3O
O ,, 0.2
0.2 g/L)
g/L)
0.99
0.99 Fit (Fe
Fit (Fe 3O
O4,, 0.2
0.2 g/L)
g/L) 3 44
3 4
0.5 Fit (Fe
(Fe3O
O ,, 0.2
0.2 g/L)
g/L)
0.95
0.95 Data (Fe
(Fe 3O
O ,, 0.3
0.3 g/L)
g/L) 0.5 Fit 3 44
Data 3 44
0.25 Data (Fe
Data (Fe 3O
O ,, 0.3
0.3 g/L)
g/L)
0.75
0.75 Fit (Fe
Fit (Fe 3O
O4,, 0.3
0.3 g/L)
g/L) 0.25 3 44
3 4 Fit (Fe
(Fe3O
O ,, 0.3
0.3 g/L)
g/L)
0.5
0.5 Data (Fe
Data (Fe 3O
O ,, 0.4
0.4 g/L)
g/L) 0.1
0.1
Fit 3 44
3 44 Data (Fe
(Fe 3O
O ,, 0.4
0.4 g/L)
g/L)
0.25
0.25 Fit (Fe
(Fe 3O
O4,, 0.4
0.4 g/L)
g/L) 0.05
0.05 Data 3 44
Fit 3 4 Fit (Fe
Fit (Fe 3O
O ,, 0.4
0.4 g/L)
g/L)
0.05
0.05 Data (Fe
Data (Fe 3O
O ,, 0.5
0.5 g/L)
g/L) 3 44
3 44
0.01
0.01 Fit (Fe
(Fe 3O
O4,, 0.5
0.5 g/L)
g/L) 0.01
0.01 Data (Fe
Data (Fe 3O
O ,, 0.5
3 44
0.5 g/L)
g/L)
Fit
0.001
3 4 0.005
0.005 Fit (Fe
(Fe3O
O ,, 0.5
0.5 g/L)
g/L)
0.001 Fit 3 44
0.0001
0.0001
0.001
0.001
0.0005
0.0005
60
60 70
70 80
80 90
90 60
60 70
70 80
80 90
90
BDV (kV)
BDV (kV) BDV (kV)
BDV (kV)
(a) (b)
Figure
Figure 11.
11. Probability plotof
Probability plot ofbreakdown
breakdownvoltage
voltagedata
dataofof SE-based
SE-based nanofluids
nanofluids with
with Fe3Fe
O43O
3 44 (20 nm)
(20 nm) for
for the 2 mm electrode gap; (a) normal and (b) extreme value.
the 2 mm electrode gap; (a) normal and (b) extreme value.
Data (SE)
(SE) Data (SE)
Data (SE)
Data
Fit (SE)
(SE) Fit (SE)
Fit (SE)
Fit
0.9999
0.9999 Data (ZnO,
Data (ZnO, 0.1
0.1 g/L)
g/L) Data (ZnO,
Data (ZnO, 0.1
0.1 g/L)
g/L)
0.999 Fit (ZnO,
(ZnO, 0.1
0.1 g/L)
g/L) 0.9999
0.9999 Fit (ZnO,
(ZnO, 0.1
0.1 g/L)
g/L)
0.999 Fit 0.995 Fit
0.995
0.995 Data (ZnO,
Data (ZnO, 0.2
0.2 g/L)
g/L) 0.995 Data (ZnO,
Data (ZnO, 0.2
0.2 g/L)
g/L)
Fit (ZnO,
(ZnO, 0.2
0.2 g/L)
g/L)
0.95
0.95 Fit (ZnO,
(ZnO, 0.2
0.2 g/L)
g/L)
Fit Fit
0.95
0.95 Data (ZnO,
(ZnO, 0.3
0.3 g/L)
g/L) 0.75
0.75 Data (ZnO,
Data (ZnO, 0.3
0.3 g/L)
g/L)
Data
0.75
Fit (ZnO,
Fit (ZnO, 0.3
0.3 g/L)
g/L) 0.5
0.5 Fit (ZnO,
Fit (ZnO, 0.3
0.3 g/L)
g/L)
0.75 Data (ZnO,
(ZnO, 0.4
0.4 g/L)
g/L) Data (ZnO,
Data (ZnO, 0.4
0.4 g/L)
g/L)
Data 0.25
0.5
0.5 Fit (ZnO,
(ZnO, 0.4
0.4 g/L)
g/L) 0.25 Fit (ZnO,
Fit (ZnO, 0.4
0.4 g/L)
g/L)
Fit
0.25
0.25 Data (ZnO,
Data (ZnO, 0.5
0.5 g/L)
g/L) 0.1 Data (ZnO,
Data (ZnO, 0.5
0.5 g/L)
g/L)
Fit (ZnO,
(ZnO, 0.5
0.5 g/L)
g/L)
0.1 Fit (ZnO,
(ZnO, 0.5
0.5 g/L)
g/L)
Fit Fit
0.05 0.05
0.05
0.05
0.005
0.005
0.001
0.001 0.01
0.01
0.0001
0.0001 0.005
0.005
0.001
0.001
0.0005
0.0005
55
55 60
60 65
65 70
70 75
75 80
80 85
85 55
55 60
60 65
65 70
70 75
75 80
80 85
85
BDV (kV)
BDV (kV) BDV (kV)
BDV (kV)
(a) (b)
Figure 12. Probability plot of breakdown voltage data of SE-based nanofluids with ZnO (25 nm) for
2 mm electrode gap; (a) normal and (b) extreme value.
2 mm electrode gap; (a) normal and (b) extreme value.
Nanomaterials 2022,
Nanomaterials 2022, 12,
2022, 12, 2105
12, 2105
2105 14 of
14 of 25
25
Nanomaterials 14 of 25
Data (SE) Data (SE)

Data (SE) Data (SE)
0.9999
0.9999 Fit (SE) Fit (SE)
Data
Fit (SE)
(SE)
Fit
Data(SE)
(SE)
0.999
0.9999
0.999 Data (ZrO 2, 0.1 g/L) 0.9999
Data
Fit
Data(SE)(ZrO , 0.1 g/L)
(ZrO 22, 0.1 g/L)
Data (ZrO 2, 0.1 g/L)
Fit (SE) 0.9999
0.995
0.995
0.999 Fit (ZrO , 0.1 g/L)
Fit (ZrO
Data
Fit (ZrO
(ZrO
, 0.1
2, 0.1
2
g/L)
, 0.1 g/L)
g/L) 0.99
0.9999
0.99
Data
Fit (ZrO
(ZrO , 0.1
2, 0.1
2 2
g/L)
g/L)
0.995
0.95 Data (ZrO
2
, 0.2 g/L) 0.9 Data
Fit (ZrO
(ZrO , 0.1 , 0.2 g/L)
g/L)
0.95 Fit
Data(ZrO
(ZrO , 0.1 g/L)
2 2, 0.2 g/L)
2
0.99
0.9 Data (ZrO
2 2, 0.2 g/L)
2
0.95 Fit (ZrO
Data (ZrO , 0.2
, 0.2g/L)
g/L) 0.9 Fit (ZrO
Data (ZrO2, 2,0.2
,0.2
0.2g/L)
g/L)
0.75 Fit (ZrO 2, 0.2
22 g/L) 0.5
0.5
Fit (ZrO g/L)
0.75 Data
Fit (ZrO(ZrO, 0.2, 0.3 g/L)
g/L) Data
2
(ZrO , 0.3
Fit (ZrO g/L)
0.5
0.75 Data (ZrO2 22, 0.3 g/L) 0.25
0.5 Data (ZrO2,22,0.20.3g/L)
g/L)
0.5 Fit (ZrO
Data (ZrO , 0.3
, 0.3g/L)
g/L)
0.25 Fit (ZrO
Data (ZrO , 0.3
, 0.3g/L)
g/L)
Fit (ZrO 2, 0.3 g/L)
0.25
0.5
0.25 2
2
0.25
0.1 Fit (ZrO 2
2, 0.3
2 g/L)
Data
Fit
Data(ZrO(ZrO
(ZrO , 0.3, 0.4 g/L)
g/L)
2 22, 0.4 g/L)
0.1 Data
g/L)
0.25 0.05
0.1
0.05
Data (ZrO2 2, 0.4 g/L)
2
0.05
0.05 Fit (ZrO
Data
Fit (ZrO
(ZrO
, 0.4
, 0.4
2, 0.4
2
g/L)
g/L)
g/L) Fit (ZrO
Data (ZrO ,20.4
, 0.4g/L)
g/L)
2 0.05 Fit (ZrO 2, 0.4
2
g/L)
0.05
0.005
Data
Fit
Data(ZrO(ZrO
(ZrO , 0.4, 0.5 g/L)
g/L)
2 22, 0.5 g/L) Data
g/L)
0.005 0.01
0.01 Data (ZrO2 2, 0.5 g/L)
2
0.001 Fit (ZrO
Data (ZrO , 0.5
, 0.5g/L)
g/L)
0.001
0.005 Fit (ZrO 2, 0.5
22 g/L) 0.005
0.01
0.005 Fit (ZrO
Data
Fit (ZrO
(ZrO
, 0.5
, 0.5
2, 0.5
2
g/L)
g/L)
g/L)
0.0001
0.001
0.0001
0.005
2
0.0001 0.001
0.001
0.0005
0.001
0.0005
0.0005
55
55 60
60 65
65 70
70 75
75 80
80 85
85 55
55 60
60 65
65 70
70 75
75 80
80 85
85
55 60 65 BDV
BDV (kV)75
70 (kV) 80 85 55 60 65 BDV (kV)75
70 (kV)
BDV 80 85
BDV (kV) BDV (kV)
(a)
(a) (b)
(b)
(a) (b)
Figure 13. Probability
Figure Probability plot
plot of breakdown
breakdown voltage data
data of SE-based
SE-based nanofluids with
with ZrO22 (20–30
(20–30 nm)
nm)
Figure 13.
13. plot of
Probability plot of breakdown voltage
of breakdown voltage data of
voltage data of SE-based nanofluids
of SE-based nanofluids with ZrO
nanofluids with ZrO22 (20–30
ZrO (20–30 nm)
nm)
for
for the
the 2 mm
22 mm electrode
electrode gap;
gap; (a)
(a) normal
normal and
and (b)
(b) extreme
extreme value.
value.
for the mm electrode gap; (a) normal and (b) extreme
for the 2 mm electrode gap; (a) normal and (b) extreme value. value.
Data (SE) Data (SE)

Data (SE) Data (SE)
0.9999
0.9999 Fit (SE) Fit (SE)
Fit (SE)
Data (SE) Data
Fit (SE)(SE)
0.999
0.9999
0.999 Data (SiO 2, 0.1 g/L) Data
Fit (SE)
Data
(SiO , 0.1 g/L)
(SiO 22, 0.1 g/L)
0.995
Data (SiO 2, 0.1 g/L)
Fit (SE) 0.9999
0.9999
0.995
0.999 Fit
Data
Fit
(SiO
(SiO
(SiO
, 0.1 g/L)
, 0.1
2, 0.1 g/L)
g/L) 0.995 Fit
Data
Fit
(SiO
(SiO(SiO , 0.1
, 0.1
2, 0.1
g/L)
g/L)
g/L)
0.995 22 0.995
0.9999 2
2
0.95 Data
Fit (SiO
(SiO , 0.2
, 0.1 g/L)
g/L) 0.95
0.95
0.995 Data
Fit (SiO(SiO, 0.1, 0.2 g/L)
g/L)
0.95 Data (SiO
2 2, 0.2 g/L)
2 Data (SiO2 2, 0.2 g/L)
2
0.95 Fit (SiO
Data
Fit (SiO
(SiO
, 0.2
, 0.2
2, 0.2
g/L)
g/L)
g/L)
0.75
0.95
0.75 Fit (SiO
Data (SiO ,20.2
, 0.2g/L)
g/L)
0.75 2
2 Fit (SiO 2, 0.2 g/L)
0.75 Data
g/L) 0.5
0.75
0.5 Data
Fit (SiO
2
(SiO, 0.2, 0.3 g/L)
g/L)
Data (SiO2 2, 0.3 g/L)
0.5
0.75
0.5 2
0.5
Data (SiO2 2, 0.3 g/L)
2
Fit (SiO
Data
Fit (SiO
(SiO
, 0.3
, 0.3
2, 0.3
2
g/L)
g/L)
g/L)
0.25
0.25 Fit (SiO
Data (SiO ,20.3
, 0.3g/L)
g/L)
0.25
0.5
0.25 2 Fit (SiO 2, 0.3
2
g/L)
Data
Fit
Data(SiO(SiO
(SiO , 0.3, 0.4
2 2, 0.4 g/L)
g/L)
g/L) 0.25
0.1 Data
g/L)
0.25 2 0.1 Data (SiO2 2, 0.4 g/L)
0.05
0.05 Fit (SiO
Data
Fit (SiO
(SiO
, 0.4
, 0.4
2, 0.4
g/L)
g/L)
g/L) 0.05
0.1 Fit (SiO
Data (SiO
2
,20.4
, 0.4g/L)
g/L)
2 2 0.05 Fit (SiO 2, 0.4 g/L)
0.05
0.005
Data
Fit
Data(SiO(SiO
(SiO , 0.4, 0.5
2 2, 0.5 g/L)
g/L)
g/L) 0.05 Data
Fit (SiO
(SiO
2
, 0.4 , 0.5 g/L)
g/L)
0.005 Fit (SiO
2
, 0.5 g/L)
Data (SiO
2 2, 0.5 g/L)
2
0.001
0.001
0.005
Data
Fit (SiO
(SiO 2
, 0.5
2, 0.5 g/L)
g/L) 0.01 Fit (SiO
Data (SiO2, 2,0.5
,0.5
0.5g/L)
g/L)
2 0.01 Fit (SiO g/L)
0.0001
0.001
0.0001
Fit (SiO 2, 0.5 g/L) 0.005
0.01
2
0.005 Fit (SiO2, 0.5 g/L)
0.0001 0.005
0.001
0.001
0.0005
0.001
0.0005
55 60 65 70 75 80 85 0.0005 55 60 65 70 75 80 85
55 60 65 70 75 80 85 55 60 65 70 75 80 85
55 60 65 BDV
BDV (kV)75
70 (kV) 80 85 55 60 65 BDV (kV)75
70 (kV)
BDV 80 85
BDV (kV) BDV (kV)
(a)
(a) (b)
(b)
(a) (b)
Figure 14.
Probability plot
plot of
of breakdown
breakdown voltage
voltage data
data of
of SE-based
SE-based nanofluids
nanofluids with
with SiO
SiO22 (10–20
(10–20 nm)
nm)
Figurethe 214.
for the 2 mm
mmProbability
electrodeplot
gap;of(a)
breakdown
(a) voltage
normal and
and data ofvalue.
(b) extreme
extreme (10–20 nm)
SE-based nanofluids with SiO22 (10–20 nm)
for electrode gap; normal (b) value.
Data (SE) Data (SE)

Data (SE) Data (SE)
Fit (SE) Fit (SE)
Fit (SE)
Data (SE) Al 2O
Al O3 (20–30
(20–30 nm)
nm) Data
Fit (SE)
(SE)
Al 2OO 3(20–30
(20–30nm)
nm) Data (Al 2O3, 0.1 g/L) Data (Al O , 0.1 g/L)
0.9999
Al 2 3
Data (Al 2O3, 0.1 g/L)
Fit (SE) 0.9999
0.9999 Al22O33 (20–30 nm) Data(SE)
Fit (Al 22O33, 0.1 g/L)
0.9999 Al 2O 3 (20–30 nm) Fit (Al
Data (Al2O
Fit (Al
O
O ,, 0.1
0.1 g/L)
g/L)
2 3,3 0.1 g/L) 0.99 Fit (Al
(Al O3,30.1
Fit (Al 2O2O
Data , 0.1g/L)
g/L)
0.999 2 3 0.9999
0.99 2
, 0.1
3
g/L)
0.9999
0.999 Data (Al 2O,30.1
Fit (Al
(Al22O
, 0.2 g/L)
O33, 0.2g/L) 0.9
0.99 Data (AlOOO , 0.2 g/L)
0.99
0.999
Data g/L) 0.9 Fit
Data(Al
(Al2 23
2 3
, 0.1 g/L)
3, 0.2 g/L)
0.99 Fit (Al
Data (Al2O
Fit (Al
O
O ,, 0.2
0.2 g/L)
g/L)
2 3,3 0.2 g/L) 0.9 Fit (Al
Data OO,30.2 g/L)
0.95 2 3 0.5 Fit (Al(Al , 0.2
2O2 3, 0.2
g/L)
g/L)
0.99
0.95 Data
Data
(Al 2O,30.2
Fit (Al
(Al22O
, 0.3 g/L)
O33, 0.3g/L)
g/L)
0.5 Data
Fit (Al
2 3
(AlOOO , 0.2, 0.3 g/L)
g/L)
0.95
0.75 Fit (Al O
O ,, 0.3
0.3 g/L)
0.25
0.5
0.25 Data (Al2 23
2 3
3, 0.3 g/L)
0.75 Data (Al2O
Fit (Al g/L)
2 3,3 0.3 g/L) Fit (Al
Data OO,30.3 g/L)
0.5 2 3 0.25 Fit (Al(Al , 0.3
2O2 3, 0.3
g/L)
g/L)
0.75
0.5 Data (Al 2O,30.3
Fit (Al
Data (Al22O
, 0.4 g/L)
O33, 0.4g/L)
g/L)
0.1
0.1 2 3
Data
Fit (Al (AlOOO , 0.3, 0.4 g/L)
g/L)
0.25
0.5
0.25 Fit (Al
Data (Al2O O
O ,, 0.4
0.4 g/L)
g/L) 0.05
0.1
0.05 Data (Al2 23
2 3
3, 0.4 g/L)
Fit (Al 2 3,3 0.4 g/L) Fit (Al
Data OO,30.4 g/L)
0.25
0.05 Data
2 3
(Al 2O,30.4
, 0.5 g/L) 0.05 Fit (Al(Al , 0.4
2O2 3, 0.4
g/L)
g/L)
0.05 Fit (Al
Data (Al22OO33, 0.5g/L)
g/L)
2 3
Data
Fit (Al (AlOOO , 0.4, 0.5 g/L)
g/L)
0.01
0.05
0.01 Fit (Al
Data (Al2O O
O ,, 0.5
0.5 g/L)
g/L)
0.01
0.01 Data (Al2 23
2 3
3, 0.5 g/L)
Fit (Al 2 3,3 0.5 g/L)
0.001
0.01
2 3 0.005
0.01
0.005 Fit (Al
Data
Fit (Al(Al
OO, 0.5, 0.5
2O2 3, 0.5
3
g/L)
g/L)
g/L)
0.001 Fit (Al 2O3, 0.5 g/L) 2 3
0.0001
0.001
0.0001 0.005 Fit (Al 2O3, 0.5 g/L)
0.0001 0.001
0.001
0.0005
0.001
0.0005
0.0005
60
60 70
70 80
80 90
90 60
60 70
70 80
80 90
90
60 BDV(kV)
70 BDV (kV)
80 90 60 70 BDV (kV)
80 90
BDV (kV)
BDV (kV) BDV (kV)
(a)
(a) (b)
(b)
(a) (b)
Figure15.
Figure 15.Probability
Probabilityplot
plotof
ofbreakdown
breakdownvoltage
voltagedata
dataof
ofSE-based
SE-basednanofluids
nanofluidswith
withAl
Al22O
O33(20–30
(20–30nm)
nm)
Figure
for the 15.
2 mmProbability
electrodeplot of breakdown
gaps; (a) normal voltage
and (b) data of SE-based
extreme value. nanofluids with Al2O3 (20–30 nm)
for the 215.
Figure mm electrodeplot
Probability gaps;
of (a) normal and
breakdown (b) extreme
voltage value. nanofluids with Al2 O3 (20–30 nm)
data of SE-based
for the 2 mm electrode gaps; (a) normal and (b) extreme value.
for the 2 mm electrode gaps; (a) normal and (b) extreme value.
Nanomaterials2022,
Nanomaterials 2022,12,
12,2105
2105 15 of 25
15 of 25
Data (SE) Data (SE)

Fit (SE) Fit (SE)
Al 2O3 (50 nm) Data (Al 2O3, 0.1 g/L) Al 2O 3 ( 50 nm) Data (Al 2O 3, 0.1 g/L)
0.9999
0.9999 Fit (Al 2O3, 0.1 g/L) 0.99 Fit (Al 2O3, 0.1 g/L)
0.999 Data (Al 2O3, 0.2 g/L) 0.9 Data (Al 2O 3, 0.2 g/L)
0.99 Fit (Al 2O3, 0.2 g/L) Fit (Al 2O3, 0.2 g/L)
0.5
0.95 Data (Al 2O3, 0.3 g/L) Data (Al 2O 3, 0.3 g/L)
0.25
0.75 Data (Al 2O3, 0.3 g/L) Fit (Al 2O3, 0.3 g/L)
0.5 Data (Al 2O3, 0.4 g/L) 0.1
Data (Al 2O 3, 0.4 g/L)
0.25 0.05
Data (Al 2O3, 0.4 g/L) Fit (Al 2O3, 0.4 g/L)
0.05 Data (Al 2O3, 0.5 g/L)
Data (Al 2O 3, 0.5 g/L)
0.01 0.01
Data (Al 2O3, 0.5 g/L)
0.005 Fit (Al 2O3, 0.5 g/L)
0.001
0.0001
0.001
0.0005
60 70 80 90 50 60 70 80 90 100
BDV (kV) BDV (kV)
(a) (b)
Figure 16. Probability plot of breakdown voltage data of SE-based nanofluids with Al2O3 (50 nm)
Figure 16. Probability plot of breakdown voltage data of SE-based nanofluids with Al2 O3 (50 nm) for
the 2 mm electrode gap; (a) normal and (b) extreme value.
It resorts from the results in Table 5a,b that the addition of the Fe3O4 (20 nm), ZnO
Table 5. The AC BDV at 1, 10, and 50% probability levels evaluated from normal and extreme value
(25 nm), ZrO2 (20–30 nm), SiO2 (10–20 nm), Al2O3 (20–30 nm), and Al2O3 (50 nm) NPs could
fit curves.
not only enhance the mean AC BDV (from 50% risk level) but also improve the AC BDV
at 1% and 10%1%
risk levels. Mainly, the addition
10%
of these NPs strongly affects
50%
the U1% rather
than U10% and U50%, exceeding 75% of improvement with Fe3O4 (20 nm) and Al2O3 (20–30
Increment Increment Increment
Concentration Concentration and
BDV50 (kV)
nm) compared to pure SE.
BDV Still,
(kV) Fe3O4 (20 nm) and AlBDV
2O3 (20–30
(kV) and 50 nm) give
(%) (%) (%)
the best U10% and U50% compared to ZnO (25 nm), ZrO2 (20–30 nm), and SiO2 (10–20 nm)
Normal NFs.49.30 - 55.90 - 64.00 -
Pure SE
EV 43.60 - 55.60 - 65.10 -
Table 5. The ACSE-based NFs
BDV at 1, 10, with Fe3 Oprobability
and 50% 4 (20 nm) levels evaluated from normal and extreme value
Normal fit curves.

69.50 40.97 75.10 34.34 81.90 27.96
(0.1 g/L)
EV 62.10 42.43 73.50 32.19 82.60 26.88
1% 10% 50%
Concentration Normal 69.70
Concentration BDV (kV) 41.37
Increment (%) 74.90
BDV (kV) 33.98
Increment (%) 81.40(kV) Increment
BDV 21.18 (%)
(0.2 g/L)
EV 64.00 46.79 74.10 33.27 82.30 26.42
Normal 49.30 – 55.90 – 64.00 –
Pure SE Normal 76.10 54.36 80.60 44.18 86.00 34.37
(0.3 g/L) EV 43.60 – 55.60 – 65.10 –
EV 69.30 58.94 78.90 41.91 86.60 33.03
SE-based NFs with Fe3O4 (20 nm)
Normal 83.70 69.77 86.90 55.45 90.80 41.87
(0.4 g/L)
EV
Normal 77.20
69.50 77.06
40.97 84.90
75.10 34.34
52.70
81.90
91.10
27.96
39.94
(0.1 g/L)
EV 62.10 42.43 73.50 32.19 82.60 26.88
Normal 79.30 60.85 83.80 49.91 89.40 39.78
(0.5 g/L) Normal 69.70 41.37 74.90 33.98 81.40 21.18
(0.2 g/L) EV 72.20 65.60 82.10 47.66 90.00 38.25
EV 64.00 46.79 74.10 33.27 82.30 26.42
Normal 76.10 54.36 80.60 44.18 86.00 34.37
(0.3 g/L) Normal 66.10 34.07 71.50 27.90 78.00 21.87
(0.1 g/L) EV 69.30 58.94 78.90 41.91 86.60 33.03
EV 55.60 27.52 68.40 23.02 78.70 20.89
Normal 83.70 69.77 86.90 55.45 90.80 41.87
(0.4 g/L) Normal 62.00 25.76 66.30 18.60 71.60 11.87
(0.2 g/L)
EV
EV 58.20
77.20 33.49
77.06 66.00
84.90 52.70
18.71
91.10
72.20
39.94
10.91
Normal 79.30 60.85 83.80 49.91 89.40 39.78
(0.5 g/L) Normal 60.20 22.10 66.50 18.96 74.20 15.93
(0.3 g/L) EV 72.20 65.60 82.10 47.66 90.00 38.25
EV 52.60 20.64 65.10 17.09 75.10 15.36
Normal 68.20 38.33 72.80 30.23 78.40 22.5
(0.4 g/L) Normal 66.10 34.07 71.50 27.90 78.00 21.87
(0.1 g/L) EV 63.90 46.56 72.40 30.22 79.20 21.66
EV 55.60 27.52 68.40 23.02 78.70 20.89
Normal 58.10 17.84 63.10 12.88 69.30 8.28
(0.5 g/L)
EV Normal 56.20 62.00 28.90 25.76 64.0066.30 18.60
15.11 71.60
70.20 11.87
7.83
(0.2 g/L)
EV 58.20 33.49 66.00 18.71 72.20 10.91
Normal 60.20 22.10 66.50 18.96 74.20 15.93
(0.3 g/L)
EV 52.60 20.64 65.10 17.09 75.10 15.36
Normal 68.20 38.33 72.80 30.23 78.40 22.5
(0.4 g/L)
EV 63.90 46.56 72.40 30.22 79.20 21.66
Table 5. Cont.
1% 10% 50%
Increment Increment Increment
Concentration Concentration BDV (kV) BDV (kV) BDV (kV)
(%) (%) (%)
Normal 57.60 16.83 64.20 14.84 72.90 13.90
(0.1 g/L)
EV 44.00 0.92 60.50 8.81 73.80 13.36
Normal 58.80 19.26 63.90 14.31 70.20 9.68
(0.2 g/L)
EV 52.10 19.50 62.50 12.41 70.90 8.91
Normal 57.90 17.44 64.50 15.38 72.70 13.59
(0.3 g/L)
EV 52.90 21.33 64.50 16.01 73.80 13.36
Normal 73.40 48.88 76.80 37.38 80.80 26.25
(0.4 g/L)
EV 68.60 57.34 75.70 36.15 81.30 24.88
Normal 64.80 31.44 70.00 25.22 76.40 19.37
(0.5 g/L)
EV 54.70 25.46 67.10 20.68 77.00 18.28
Normal 66.40 34.68 70.60 26.29 75.80 18.43
(0.1 g/L)
EV 63.00 44.50 70.50 26.80 76.40 17.36
Normal 62.50 26.77 67.90 21.46 74.60 16.56
(0.2 g/L)
EV 54.10 24.08 65.90 18.53 75.30 15.67
Normal 68.70 39.35 73.60 31.66 79.60 24.35
(0.3 g/L)
EV 61.80 41.74 72.10 29.68 80.30 23.35
Normal 67.00 35.90 71.00 27.01 76.00 18.75
(0.4 g/L)
EV 58.10 33.26 68.30 22.84 76.40 17.36
Normal 64.10 30.02 69.10 23.61 75.30 17.65
(0.5 g/L)
EV 55.50 27.29 66.80 20.14 75.90 16.59
SE-based NFs with Al2 O3 (20–30 nm)
Normal 68.30 38.53 74.40 33.09 81.90 27.96
(0.1 g/L)
EV 62.60 43.58 73.80 32.73 82.80 27.19
Normal 68.30 38.53 82.00 46.69 86.70 35.46
(0.2 g/L)
EV 72.40 66.06 80.60 44.96 87.20 33.95
Normal 82.70 67.74 87.40 56.35 93.20 45.62
(0.3 g/L)
EV 79.80 83.03 87.70 57.73 94.00 44.39
Normal 84.50 71.39 87.70 56.88 91.60 43.125
(0.4 g/L)
EV 82.40 88.99 87.80 57.91 92.10 41.47
Normal 72.00 46.04 78.70 40.78 87.00 35.93
(0.5 g/L)
EV 65.10 49.31 77.80 39.93 88.10 35.33
SE-based NFs with Al2 O3 (50 nm)
Normal 70.30 42.59 74.20 32.73 78.80 23.12
(0.1 g/L)
EV 62.70 43.81 71.90 29.32 79.20 21.66
Normal 76.00 54.15 79.50 42.21 83.90 31.09
(0.2 g/L)
EV 70.90 62.61 78.40 41.01 84.40 29.65
Normal 76.90 55.98 83.20 48.83 91.00 42.18
(0.3 g/L)
EV 72.30 65.83 83.30 49.82 92.00 41.32
Normal 83.00 68.35 87.40 56.35 92.70 44.84
(0.4 g/L)
EV 79.10 81.42 87.10 56.65 93.40 43.47
Normal 81.80 65.92 86.70 55.09 92.60 44.68
(0.5 g/L)
EV 80.10 83.72 87.50 57.37 93.40 43.47
3.4.2. Statistical Analysis of AC Breakdown Voltage Outcomes for 2.5 mm Gap Distance
Following the same steps presented in the previous subsection, the p-value for the
EV, normal, and Weibull distributions were calculated and compared to the significance
level for AC BDV data for 2.5 mm electrode gap (Table 6). The concerned NPs are ZnO
(25 nm), ZrO2 (20–30 nm), and SiO2 (10–20 nm). It was noted that the p-value is higher
Nanomaterials 2022, 12, 2105 than the significance level for all cases except ZrO2 (20–30 nm) NF at 0.1 g/L 18
with
of 25normal
distribution, and therefore, most of the experimental data obey the three distributions.
Table 6. Hypothesis
Normal 85.00 test of 21.95
conformity of88.20
breakdown voltage
16.67 outcomes of various11.65
92.00 nanofluids to EV,
(0.4 g/L) Normal, and 81.30
EV Weibull distributions 87.50 p-value17.29
27.62 considering calculation, for 2.5 mm electrode
92.50 11.04 gaps.
Normal 79.00 13.34 83.30 10.47 88.60 7.52
(0.5 g/L) EV Normal Weibull
EV 73.40 15.22 82.20 10.18 89.30 7.202
Concentration p-Value Decision p-Value Decision p-Value Decision
Pure SE 0.5275
Normal Accepted
71.80 0.5750
3.01 77.80 Accepted
3.18 0.5733
85.30 3.51Accepted
(0.1 g/L) SE-based NFs
EV 66.90 5.02with ZnO77.70
(25 nm) 4.150 86.30 3.601
(0.1 g/L) 0.7823
Normal Accepted
76.80 0.9705
10.18 81.80 Accepted8.48 0.8702
87.90 6.67Accepted
(0.2 g/L)
(0.2 g/L) 0.3589 EV Accepted 0.2998 0.3613
73.50 15.38 82.00 Accepted
9.910 88.80 6.602Accepted
(0.4 g/L) Normal
0.6970 81.70
Accepted 17.21
0.6941 85.50 13.39
Accepted 90.10
0.7461 9.34 Accepted
(0.3 g/L)
(0.5 g/L) 0.4051 EV 76.40
Accepted 19.93
0.8049 84.30 Accepted
13.00 90.70
0.4919 8.883Accepted
Normal 83.00
SE-based NFs 19.08 87.00 nm) 15.38
with ZrO2 (20–30 91.80 11.40
(0.4 g/L)
(0.1 g/L) 0.0565 EV 78.70
Accepted 23.54
0.0438 86.30Not-Accepted
15.68 92.40
(0.2 g/L) Normal
0.5412 78.50
Accepted 12.62
0.3017 83.30 Accepted
10.47 89.20
0.5162 8.25Accepted
(0.5 g/L)
(0.3 g/L) 0.1277 EV Accepted 0.5189 0.1612
73.10 14.75 81.60 Accepted
9.400 89.90 7.923Accepted
(0.5 g/L) 0.5753 Accepted with SiO2 (25 nm)
SE-based NFs0.8512 Accepted 0.6822 Accepted
Normal 76.80 10.18 81.90 8.62 88.10 6.91
(0.1 g/L) SE-based NFs with SiO2 (10–20 nm)
EV 71.60 12.40 81.20 8.84 88.90 6.722
(0.2 g/L) Normal
0.7526 78.10
Accepted 12.05
0.3288 83.40 10.61
Accepted 89.80
0.7011 8.98Accepted
(0.2 g/L)
(0.3 g/L) 0.8697 EV 75.10
Accepted 17.89
0.7511 83.70 Accepted
12.19 90.70
(0.4 g/L) 0.1784
Normal Accepted
86.10 0.5097
23.52 89.30 Accepted
18.43 0.2118
93.30 13.22Accepted
(0.3 g/L)
EV 82.60 29.67 88.80 19.03 93.70 12.48
Normal 82.00 17.64 84.90 12.59 88.50 7.40
(0.4 g/L)
EV Figures77.50 21.66 the normal
17 and 18 show 83.90and EV 12.46 88.90
probability density plot 6.722
of ZnO (25 nm),
Normal
ZrO2 (20–3075.00
nm), and SiO 7.60
2 (10–20 nm)79.10
NFs versus4.90
AC BDV for 84.20 2.18
different concentrations.
(0.5 g/L)
EV From those70.10 plots, the
10.04 78.30
BDV at risk levels (1%,4.95 84.90 are evaluated
10%, and 50%) 1.920 and pre-
sented in Table 7. Like those for 2 mm electrode gaps, those results for 2.5 mm show that
In addition,
the addition of ZnOthe (25
concentrations
nm), ZrO2 for the optimal
(20–30 increments
nm), and are identical
SiO2 (10–20 nm) NPs to those
couldthat
not only
give the best mean AC BDV. This observation could easily be verified in
enhance the mean AC BDV but also improve the AC BDV at 1% and 10% risk levels. Figures 17–19Mainly,
below, where the line corresponding to the optimal concentrations is in the right of the
NPs’ addition affects the U1% more than U10% and U50% , exceeding 25% of improvement
others, whatever the breakdown probability.
with the three NFs compared to pure SE.
Data (SE) Data (SE)

0.995 Fit (SE) 0.9999 Fit (SE)
Data (ZnO, 0.1 g/L) 0.995 Data (ZnO, 0.1 g/L)
0.95 Fit (ZnO, 0.1 g/L) 0.95 Fit (ZnO, 0.1 g/L)
Data (ZnO, 0.2 g/L) Data (ZnO, 0.2 g/L)
0.75 Fit (ZnO, 0.2 g/L)
0.75 Fit (ZnO, 0.2 g/L)
Data (ZnO, 0.3 g/L) 0.5 Data (ZnO, 0.3 g/L)
0.5 Fit (ZnO, 0.3 g/L)
Fit (ZnO, 0.3 g/L)
0.25 0.25 Data (ZnO, 0.4 g/L)
Data (ZnO, 0.4 g/L)
Fit (ZnO, 0.4 g/L) Fit (ZnO, 0.4 g/L)
0.1 Data (ZnO, 0.5 g/L)
0.05 Data (ZnO, 0.5 g/L)
Fit (ZnO, 0.5 g/L) 0.05 Fit (ZnO, 0.5 g/L)
0.005
0.0005 0.01
0.0001 0.005
0.001
0.0005
75 80 85 90 95 75 80 85 90 95
BDV (kV) BDV (kV)
(a) (b)
Figure Probability
17.electrode
2.5 mm plot
gaps; of breakdown
(a) normal voltagevalue.
and (b) extreme data of SE-based nanofluids with ZnO (25 nm) for
2.5 mm electrode gaps; (a) normal and (b) extreme value.
18 of 25
Data (ZrO 2, 0.1 g/L) Data (SE)

0.995 Fit (SE)
Fit (ZrO , 0.1 g/L)
2
0.9999
Data (ZrO 2, 0.2 g/L) 0.995
0.95 0.95
0.9 Fit (ZrO2, 0.2 g/L)
0.75 Data (ZrO 2, 0.3 g/L) 0.75
Fit (ZrO2, 0.3 g/L) 0.5
0.5 Data (ZrO 2, 0.3 g/L)
Data (ZrO , 0.4 g/L)
0.25
2
0.25 Fit (ZrO 2, 0.3 g/L)
Fit (ZrO2, 0.4 g/L)
0.1 Data (ZrO , 0.5 g/L) 0.1
0.05 2 Fit (ZrO 2, 0.4 g/L)
Fit (ZrO , 0.5 g/L) 0.05
2
0.005 Data (SE)
Fit (SE) Fit (ZrO 2, 0.5 g/L)
0.0005 0.01
0.0001
0.005
75 80 85 90 95 75 80 85 90 95
BDV (kV) BDV (kV)
(a) (b)
Figure 18. Probability plot of breakdown voltage data of SE-based nanofluids with ZrO2 (20–30 nm)
for 2.5 mm electrode gaps; (a) normal and (b) extreme value.
Data (SE)
0.9999 Table 7. The AC BDV atData
1,(SE)10, and 50%
Fit (SE) 0.9999probability levels evaluated from normal and extreme value
Fit (SE)
0.999 0.995 Data (SiO , 0.1 g/L)
Data (SiO , 0.1 g/L)
0.995 fit curves. Fit (SiO ,0.1 g/L) 0.95
2
Fit (SiO , 0.1 g/L)
2
2 2
0.95 Data (SiO2, 0.2 g/L) 0.75 Data (SiO 2, 0.2 g/L)
0.75 Fit (SiO 2,0.2 g/L) 0.5 Fit (SiO 2 , 0.2 g/L)
1% Data (SiO2, 0.3 g/L)
10% 50%
Data (SiO 2, 0.3 g/L)
0.5 0.25
Fit (SiO , 0.3 g/L)
Concentration
0.25 Distribution BDV (kV) Increment (%)
2 BDV (kV) Increment (%) BDV (kV)Fit (SiO , 0.3Increment
g/L)
2 (%)
Data (SiO2, 0.4 g/L) 0.1 Data (SiO 2, 0.4 g/L)
0.05 Normal 69.70 -
Fit (SiO 2, 0.4 g/L) 0.05 75.40 - 82.40 Fit (SiO 2 , 0.4 g/L) -
Pure SE 0.005 EV 63.70 Data (SiO2, 0.5 g/L)
- 74.60 - 83.30 Data (SiO 2, 0.5 g/L) -
0.001 Fit (SiO 2, 0.5 g/L) Fit (SiO 2 , 0.5 g/L)
0.01
0.0001 SE-based NFs with 0.005
ZnO (25 nm)
(0.1 g/L) Normal 77.40 11.04 81.90 8.62 87.30 5.94

EV 72.10 13.18 0.00180.90 8.440 88.00 5.642
75 80
Normal 85 90
79.90 95 14.63 75
84.20 80 85
11.67 90 9589.60 8.73
(0.2 g/L) BDV (kV) BDV (kV)
EV 75.10 17.89 83.50 11.93 90.30 8.403
Normal (a)82.70 18.65 86.10 14.19(b) 90.30 9.58
(0.3 g/L)
EV 80.70 26.68 86.40 15.81 90.90 9.123
Figure 19. Probability plot of breakdown voltage data of SE-based nanofluids with SiO2 (10–20 nm)
(0.4 g/L) Normal for 85.00 21.95 (a) normal and
2.5 mm electrode gaps; 88.20 16.67
(b) extreme value. 92.00 11.65
EV 81.30 27.62 87.50 17.29 92.50 11.04
(0.5 g/L) Normal 79.00

3.5.73.40 13.34
Partial Discharge15.22 83.30
Activity of Al2O382.20 10.47
and Fe3O4 NFs 10.18 88.60 7.52
EV 89.30 7.202
Table 8 presents
SE-based the
NFsaverage
with ZrOand standard deviation (St. Dev), as well as the incre-
2 (20–30 nm)
ment percentage of PDIV (partial discharge inception voltage), PDEV (partial discharge
(0.1 g/L) Normal 71.80 3.01 77.80 3.18 85.30 3.51
EV extinction
66.90 voltage), Q avg, Qpeak, and NPDs/s
5.02 77.70 values obtained
4.150 from electrical
86.30 measurements 3.601
Normal for76.80
different liquids10.18
tested with a threshold
81.80 detection8.48
level of 500 fC. This
87.90threshold is just
6.67
(0.2 g/L)
EV above
73.50the background
15.38noise and allows
82.00 the PD activity
9.910comparison of the four liquids
88.80 at
6.602
Normal the81.70
same voltage level.
17.21The higher applied
85.50 voltage than 13 kV RMS could
13.39 90.10 lead to the pure
9.34
(0.3 g/L)
EV SE 76.40
breakdown and 19.93 84.30 higher than13.00
for a threshold level 500 fC, the PDIV90.70
and PDEV voltage 8.883
(0.4 g/L) Normal 83.00

could 19.08in the case of87.00
not be measured Al2O3 NFs. 15.38 91.80 11.40
EV 78.70 23.54 86.30 15.68 92.40 10.92
(0.5 g/L) Normal 78.50

Table 8. PD activity of12.62 83.30
synthetic ester and 10.47 nanofluids with
synthetic ester-based 89.20Fe3O4 (20 nm) and
8.25
EV 73.10
Al2O 14.75
3 (20–30 and 50 nm).
81.60 9.400 89.90 7.923
Fe3O4 (20 nm) NF Al2O3 (20–30 nm) NF Al2O3 (50 nm) NF
(0.1 g/L) Normal Pure SE76.80
MIDEL 7131 10.18 81.90 8.62 88.10 6.91
EV 71.60 12.40 at 0.4 g/L 81.20 at 0.3
8.84g/L 88.90 at 0.4 g/L 6.722
PDIV (kV)Normal 10.286
78.10 12.05 12.647 83.40 12.815
10.61 89.80 12.77 8.98
(0.2 g/L)
St. Dev (kV)EV 75.10
0.763 17.89 1.0435 83.70 12.19
0.511 90.70 0.325 8.883
Increment Normal
(0.3 g/L) (%) 86.10
– 23.52 22.95 89.30 18.43
24.58 93.30 24.14 13.22
EV 82.60 29.67 88.80 19.03 93.70 12.48
PDEV (kV) 8.9226 11.840 10.243 11.48
Normal
(0.4 g/L)St. Dev (kV) 82.00 17.64 84.90 12.59 88.50 7.40
EV 2.1567
77.50 21.66 0.9922 83.90 1.352
12.46 88.90 1.054 6.722
Increment Normal
(%) –
75.00 7.60 32.69 79.10 14.79
4.90 84.20 28.66 2.18
(0.5 g/L)
EV 70.10 10.04 78.30 4.95 84.90 1.920
In addition, the concentrations for the optimal increments are identical to those that
give the best mean AC BDV. This observation could easily be verified in Figures 17–19
Fit (ZrO , 0.5 g/L) 0.05
2
0.005 Data (SE)
Fit (SE) Fit (ZrO 2, 0.5 g/L)
0.0005 0.01
0.0001
0.005
75 80 85 90 95 75 80 85 90 95
Nanomaterials 2022, 12, 2105 BDV (kV) BDV (kV) 19 of 25
(a) (b)
below, where the line corresponding to the optimal concentrations is in the right of the
others, whatever the breakdown probability.
Data (SE)
0.9999 Data (SE)
Fit (SE) 0.9999 Fit (SE)
0.999 0.995 Data (SiO 2, 0.1 g/L)
Data (SiO2, 0.1 g/L)
0.995
Fit (SiO 2,0.1 g/L) 0.95 Fit (SiO 2 , 0.1 g/L)
0.95 Data (SiO2, 0.2 g/L) 0.75 Data (SiO 2, 0.2 g/L)
0.75 Fit (SiO 2,0.2 g/L) 0.5 Fit (SiO 2 , 0.2 g/L)
Data (SiO2, 0.3 g/L) Data (SiO 2, 0.3 g/L)
0.5 0.25
Fit (SiO 2, 0.3 g/L) Fit (SiO 2 , 0.3 g/L)
0.25
Data (SiO2, 0.4 g/L) 0.1 Data (SiO 2, 0.4 g/L)
0.05 Fit (SiO 2, 0.4 g/L) 0.05 Fit (SiO 2 , 0.4 g/L)
Data (SiO2, 0.5 g/L)
0.005 Data (SiO 2, 0.5 g/L)
0.001 Fit (SiO 2, 0.5 g/L) Fit (SiO 2 , 0.5 g/L)
0.01
0.0001
0.005
0.001
75 80 85 90 95 75 80 85 90 95
BDV (kV) BDV (kV)
(a) (b)
Figure
Figure 19.
19. Probability
Probability plot
plot of
of breakdown
breakdown voltage
voltage data
data of
of SE-based
SE-based nanofluids
nanofluids with
with SiO
SiO22 (10–20
(10–20 nm)
nm)
3.5. Partial Discharge Activity of Al22O O33and

andFe
Fe33OO4 4NFs
NFs
Table 8 presents the average and standard
Table 8 presents the average and standard deviation deviation(St.(St. Dev),
Dev), as well
as well as increment
as the the incre-
ment percentage
percentage of PDIV of(partial
PDIV (partial
discharge discharge
inceptioninception
voltage),voltage), PDEVdischarge
PDEV (partial (partial discharge
extinction
extinction
voltage), Q voltage), Qavg
avg , Qpeak , Qpeak
, and , and NPDs/s
NPDs/s valuesvalues obtained
obtained fromfrom electrical
electrical measurements
measurements for
for different
different liquids
liquids tested
tested with
with a threshold
a threshold detectionlevel
detection levelofof500
500fC.
fC.This
Thisthreshold
threshold is just
above the background noise and allows the PD activity comparison of the four liquids at
the same voltage level. The higher applied voltage than 13 kV RMS could lead to the pure
SE breakdown and for a threshold level higher than 500 fC, the PDIV and PDEV voltage
could not be measured in the case of Al2O33 NFs. NFs.
Table 8.
Table 8. PD activity of synthetic
synthetic ester
ester and
and synthetic
ester-based nanofluids
nanofluids with
with Fe
Fe33O4 (20 nm) and
Al22O
O33 (20–30
(20–30and
and50
50nm).
nm).
Pure Fe3Fe
O43O 4 (20 nm) NF
(20 nm) NF Al2(20–30
Al2 O O3 (20–30 nm) NF
nm) NF Al2Al
O32O 3 (50 nm) NF
(50 nm) NF
Pure SESE MIDEL
MIDEL 71317131 at 0.4
3
at 0.4 g/L g/L at 0.3atg/L
0.3 g/L at 0.4
at 0.4 g/L g/L
PDIV(kV)
PDIV (kV) 10.286
10.286 12.647
12.647 12.815
12.815 12.77
12.77
St.Dev
St. Dev(kV)
(kV) 0.763
0.763 1.0435
1.0435 0.5110.511 0.325
0.325
Increment
Increment(%)
(%) - – 22.95
22.95 24.5824.58 24.14
24.14
PDEV(kV)
PDEV (kV) 8.9226
8.9226 11.840
11.840 10.243
10.243 11.48
11.48
St.
St.Dev
Dev(kV)
(kV) 2.1567
2.1567 0.9922
0.9922 1.3521.352 1.054
1.054
Increment (%) - 32.69 14.79 28.66
Increment (%) – 32.69 14.79 28.66
Qavr (pC) 123.8 3.30 3.933 4.15
St. Dev (pC) 20.06 1.574 0.377 5.864
Increment (%) - −97.33 −96.82 −96.64
Qpeak (pC) 740.44 122.68 48.95 510.6
St. Dev (pC) 49.250 97.07 29.23 104.20
Increment (%) - −83.43 −93.38 −31.04
NPDs/s (PDs/s) 9.20 1.00 1.16 1.16
St. Dev (PDs/s) 27.686 0.00 0.408 0.408
Increment (%) - −93.92 −90.14 −86.52
The PDIVs and PDEVs values of SE-based NFs are higher than those in pure SE
in all cases. With 0.3 g/L Al2 O3 (20–30 nm) NPs, the PDIV was enhanced by 24.58%,
while 0.4 g/L Fe3 O4 (20 nm) and Al2 O3 (50 nm) NPs enhanced it by 22.95% and 24.14%,
respectively. A similar tendency was observed with PDEV, i.e., 32.69%, 14.79%, and 28.66%
NPDs/s (PDs/s) 9.20 1.00 1.16 1.16
St. Dev (PDs/s) 27.686 0.00 0.408 0.408
Increment (%) – −93.92 −90.14 −86.52
Nanomaterials 2022, 12, 2105 The PDIVs and PDEVs values of SE-based NFs are higher than those in pure SE 20 of
in25all
cases. With 0.3 g/L Al2O3 (20–30 nm) NPs, the PDIV was enhanced by 24.58%, while 0.4
g/L Fe3O4 (20 nm) and Al2O3 (50 nm) NPs enhanced it by 22.95% and 24.14%, respectively.
ofAimprovement
similar tendency wascase
in the observed
of Fe3with PDEV,
O4 (20 nm),i.e.,
Al32.69%, 14.79%,
2 O3 (20–30 nm),and and28.66%
Al2 Oof improve-
3 (50 nm),
ment in theFurthermore,
respectively. case of Fe3O4 a(20 nm),QAl
lower avg2O
,Q3 (20–30 nm),
peak , and and Alfor
NPDs/s 2Othe
3 (50 nm),NFs
three respectively.
than pure Fur-
SE
thermore,
was observed.a lower Qavg, Qpeak, and NPDs/s for the three NFs than pure SE was observed.
Figures20–23
Figures 20–23showshowthethe PDs
PDs patterns of of pure
pure SE,
SE,SE-based
SE-basedFeFe 3O 4 (20
3O nm),
4 (20 Al2Al
nm), O32 O
(20–
3
30 nm),
(20–30 andand
nm), Al2O
Al3 2(50
O3 nm)
(50 NFs, respectively,
nm) NFs, at 13 kV
respectively, (RMS)
at 13 voltagevoltage
kV (RMS) level. Itlevel.
was observed
It was
that the that
observed PDs the
activity starts with
PDs activity thewith
starts appearance of PDs at
the appearance of the
PDspeak
at theofpeak
negative polarity
of negative
polarity ◦
(270 electrical degrees) anda just
(270° electrical degrees) and just few acycles
few cycles
later later
at theatpeak
the peak of positive
of positive polarity
polarity (90°
(90 ◦ electrical degrees). Except for Fe O (20 nm) NF, a smaller number of PDs was
electrical degrees). Except for Fe3O4 (203 nm) 4 NF, a smaller number of PDs was noticed in
noticed in thepolarity
the positive positivethanpolarity
in thethan in thebut
negative, negative, but with
with a higher a higher
charge charge
level for purelevel
SE, Alfor
2O3
pure SE, nm),
(20–30 Al2 Oand
3 (20–30
Al2Onm),
3 (50 and
nm)Al 2 O3 The
NFs. (50 nm)
Fe3ONFs.
4 (20 The
nm)Fe NF3 Omanifests
4 (20 nm) NF the manifests the
lowest/highest
lowest/highest activity
activity in negative andinpositive
negativepolarities,
and positive polarities,unlike
respectively, respectively, unlike other NFs.
other NFs.

Figure 20. PD pattern of pure synthetic ester (MIDEL 7131) at 13 kV (RMS) voltage level.
Figure 20. PD pattern of pure synthetic ester (MIDEL 7131) at 13 kV (RMS) voltage level.
Figure 21. PD pattern of synthetic ester-based NF with Fe3O4 (20 nm, 0.4 g/L) at 13 kV (RMS) voltage
Figure 21. PD pattern of synthetic ester-based NF with Fe3 O4 (20 nm, 0.4 g/L) at 13 kV (RMS)
level.
voltage level.
Figure 21. PD pattern of synthetic ester-based NF with Fe3O4 (20 nm, 0.4 g/L) at 13 kV (RMS) voltage
Figure
level. 21. PD pattern of synthetic ester-based NF with Fe3O4 (20 nm, 0.4 g/L) at 13 kV (RMS) voltage
level.
Figure
22.22.
PDPD pattern
pattern ofof synthetic
ester-based NFNF with
with AlAl 2O3 (20–30 nm, 0.3 g/L) at 13 kV (RMS)
Figure 2 O3 (20–30 nm, 0.3 g/L) at 13 kV (RMS)
Figure
voltage22. PD pattern of synthetic ester-based NF with Al
level. 2O3 (20–30 nm, 0.3 g/L) at 13 kV (RMS)
voltage
voltagelevel.
level.
Figure 23. PD pattern of synthetic ester-based NF with Al2O3 (50 nm, 0.4 g/L) at 13 kV (RMS) voltage
Figure 23. PD
level. 23. PD pattern
pattern of
ofsynthetic
syntheticester-based
ester-basedNF
NFwith
withAl2Al
O3 O(50 nm, 0.4 g/L) at 13 kV (RMS) voltage
Figure 2 3 (50 nm, 0.4 g/L) at 13 kV (RMS)
level.
voltage level.
4. Discussion
Statistical analysis was performed on the AC BDV outcomes at 2 mm and 2.5 mm
electrode gaps, and conformity to EV, normal, and Weibull statistical laws were conducted
based on the p-value calculation. In other words, the AD statistics were employed to
compute the corresponding p-value for each sample and compare it to the significance level.
The results show that the experimental data of breakdown voltages for SE and SE-based
Fe3 O4 (20nm), ZnO (25 nm), ZrO2 (20–30 nm), SiO2 (10–20 nm), Al2 O3 (20–30 nm), and
Al2 O3 (50 nm) NPs mostly obey EV, normal, and Weibull distributions.
On the other hand, Fe3 O4 (20 nm), ZnO (25 nm), ZrO2 (20–30 nm), SiO2 (10–20 nm),
and Al2 O3 (20–30 and 50 nm) NPs have a significant improvement of the AC breakdown
voltage (AC BDV) of synthetic ester, MIDEL 7131. Furthermore, the BDV test was carried
out for all NPs with a 2 mm electrode gap because of the breakdown voltage of Fe3 O4
(20 nm) Al2 O3 (20–30 and 50 nm) NFs for a 2.5 mm electrode gap exceeds the tester’s
voltage limitation, which is 100 kV. For the 2 mm electrode gaps, SiO2 (10–20 nm) and
Al2 O3 (20–30 nm) NPs give the best improvements at a concentration of 0.3 g/L, while the
best improvements with Fe3 O4 (20 nm), ZnO (25 nm), ZrO2 (20–30 nm), and Al2 O3 (50 nm)
NPs are observed with a concentration 0.4 g/L. Similar results have been reported by other
researchers [14,16,17,31].
The fact that there is an optimal concentration of NPs could be due to the saturation of
the NPs/SE interfaces [16]; hence, the smaller particles may show their best AC BDV at
lower concentrations than bigger particles. Beyond optimal concentration, an additional
amount of NPs will show a lower or even negative effect on the AC BDV. Accordingly, up
to 0.3 g/L, a slightly lower mean AC BDV has been observed with Al2 O3 (50 nm) than with
Al2 O3 (20–30 nm); a reversed tendency is observed beyond 0.4 g/L. Khaled and Beroual
reported a similar tendency with mineral oil and SE [16]. With Fe3 O4 (20 nm), ZnO (25 nm),
ZrO2 (20–30 nm), and Al2 O3 (50 nm) NFs, the best enhancements are about 37.70%, 19.38%,
21.37%, and 42.13%, respectively, while there are about 20.30% and 44.12% in the case of
SiO2 (10–20 nm) and Al2 O3 (20–30 nm) NFs, respectively, compared to pure SE. From the
results presented above, Fe3 O4 (20 nm) and Al2 O3 (20–30 nm and 50 nm) NFs show the
best performances according to AC BDV results. The best improvements are greater than
35% for all cases.
Nevertheless, a minor decline in AC BDV of ZnO (25 nm), ZrO2 (20–30 nm), and SiO2
(10–20 nm) NFs is observed after modifying the electrodes gap to 2.5 mm. Furthermore,
the optimal concentrations of those NPs are confirmed, 0.4 g/L for ZnO (25 nm), ZrO2
(20–30 nm) and NPs, and 0.3 g/L for SiO2 (10–20 nm) NPs, which give 14.28%, 11.13%, and
12.83% of improvements compared to SE, respectively.
Khaled and Beroual [16] examined the same SE MIDEL 7131 with Fe3 O4 (50 nm), SiO2
(10–20 nm), and Al2 O3 (13 and 50 nm) NPs. They reported that the best improvements in
breakdown voltages are obtained with Fe3 O4 and SiO2 NFs at the maximum concentration
of 0.4 g/L (upper limit, no optimal concentration), with Al2 O3 (50 nm) NF at 0.3 g/L
(optimal concentration), and, at 0.05 g/L (lower limit, minimum concentration) with Al2 O3
(13 nm) NF. Their work suggests that the smaller the NPs, the higher AC BDV is (for the
same concentration). The best improvement with SiO2 NF is about 30% compared to pure
SE, while in the present work, the optimal improvement is about 11.62% at 0.3 g/L (for
2.5 mm electrode gap). In addition, they reported a lower AC BDV breakdown voltage
for a MIDEL 7131 (60 kV) compared to the results in this work (82.6 kV); likely, this is
likely because they have been used an aged MIDEL 7131. The same authors investigated
the effect of conductive NPs (Fe3 O4 ) on the AC BDV of mineral oil, synthetic and natural
Esters-based NFs [34]. Their findings reveal that Fe3 O4 nanoparticles significantly improve
AC BDV of mineral oil (MO) and synthetic ester (SE). These improvements are 100% and
48% with MO and SE-based NFs, respectively. The improvement does not exceed 7% with
natural ester, unlike MO and SE, even reducing the AC BDV.
Different mechanisms have been proposed to describe the processes associated with
a dielectric strength enhancement when adding a small amount of NPs to host liquids.
Hwang et al. [11] introduced the electron scavenging model as a possible mechanism that
depends on the relaxation time constant (τr ). It well describes the enhancement of the
insulating performances of base liquid with addressed conductive NPs (Fe3 O4 ), but it fails
to explain the performance improvement of other NPs, even conductive ones [18]. The
mechanisms by which conductive, semi-conductive, and dielectric NPs trap electrons are
explained by the potential well distribution caused by induced or polarized charges [10].
The difference between conductivity or permittivity of NPs and host liquid could generate
induced and/or polarized charges on the NPs/SE interface, producing electrons trapping
site [10]. The formed trapping site on the interface could trap moving electrons, enhancing
the base liquid’s breakdown performance.
The involved mechanisms in enhancing BDV of NFs could also be discussed by
considering the behavior of spherical particles (roughly assuming that the particles are
spherical) suspended in a liquid and subjected to a uniform applied electric field; three
cases are possible.
The first case is when the polarizability of the NP is more significant than the base
liquid. That means that there are more charges inside the interface (NP side) than outside
(liquid side), resulting in a surface charge density difference on both sides of the interface.
So, an induced dipole is aligned with the field applied through the particle [35]. A suitable
example of this case would be a conducting NP (or NP ‘insulting or conducting’ with a
high dielectric constant) in an insulating liquid with a low dielectric constant.
The second case is when the polarizability of the NP is less significant than the base
liquid, which means that there are fewer charges inside the interface (NP side) than outside
(liquid side). The resulted dipole points in the opposite direction. This could be an
insulating NP suspended in a liquid with a high dielectric constant or high conductivity.
The third case is when the polarizability of the NP and that of the liquid are the same,
and there is no net dipole. Obviously, the second and the third cases do not correspond
to our study since, in most cases, the NPs conductivity and/or permittivity is higher than
that of SE.
Nevertheless, the charge polarized on the surface of the NP produces the trap-
ping site (potential well) [10]. Electron trapping by NPs significantly slows down the
streamer’s development by reducing its velocity and enhancing the NFs breakdown volt-
age. Sima et al. [10] conducted studies investigating the depth of the potential well of
conducting Fe3 O4 , semi-conductive TiO2 , and insulating Al2 O3 NPs. They found that the
potential wells of dielectric NPs are shallower than those of conductive NPs [10].
The results from the performed PDs test on Fe3 O4 (20 nm), Al2 O3 (20–30 nm), and
Al2 O3 (50 nm) nanofluids at optimal concentrations show a considerable enhancement of
PDs resistivity of pure SE. Alike, it was found that the PD inception voltage (PDIV), PD
extinction voltage (PDEV) are pushed to higher voltage levels when adding Fe3 O4 (20 nm),
Al2 O3 (20–30 nm), and Al2 O3 (50 nm) NPs to the reference SE under AC stress. Also, those
NFs show a reduced Qavg , Qpeak , and NPDs/s compared to SE.
According to Atiya et al. [24], the thickness of the electrical double layer (EDL) around
NP plays a vital role in reducing PD activity; the thicker the EDL, the more resistive to
PD. However, in our case, the zeta potential measurements show that Al2 O3 (50 nm) NPs
show a higher zeta potential than Fe3 O4 (20 nm) and Al2 O3 (20–30 nm) NPs; hence the
EDL thickness for Al2 O3 (50 nm) NPs is larger than that for Al2 O3 (20–30 nm) and Fe3 O4
(20 nm) NPs [24].
Depending on the properties of the NPs and the liquid used, the presence of NPs
can induce electric field heterogeneity in the NF. The localized increase of the electric
field can lead to PDs at the same applied voltage or at the same ionization level of the
liquid. Thus, near the electrodes, high mobility electrons and low mobility ionized ions
are ready to migrate under the electric field forces. The NPs then play the role of electrons
and negative ion scavengers, which generate a potential well (trapping site) that reduces
the electron/negative ion movement and thence PD activities [10,36]. When the trapping
process is finished, nanoparticle surfaces are saturated with negative charges; hence they
no longer could trap more electrons. The limit is strongly correlated with the mismatch
between base liquid and NP’s conductivities and/or permittivities [10,35].
5. Conclusions
In this work, it was shown that the AC breakdown voltage of synthetic ester-based
ZrO2 (20–30 nm), ZnO (25 nm), SiO2 (10–20 nm), Al2 O3 (20–30 nm), Al2 O3 (50 nm), and
Fe3 O4 (20 nm) nanofluids are improved. The improvements are the best with conductive
nanoparticles (Fe3 O4 ) and insulating nanoparticles (Al2 O3 ), regardless of the size. How-
ever, the addition of insulating nanoparticles (Al2 O3 ) with the smallest size (20–30 nm)
shows the best improvement at a lower concentration. The statistical analysis of the
experimental results shows that the breakdown voltage outcomes mostly obey the EV,
normal, and Weibull distributions. Additionally, it has been shown that the addition of
Al2 O3 (20–30 nm), Al2 O3 (50 nm), and Fe3 O4 (20 nm) NPs significantly reduces the partial
discharge activity compared to pure SE.
Author Contributions: Conceptualization, H.K., A.B. and E.V.; methodology, H.K., A.B. and E.V.;
software, H.K.; validation, A.B. and E.V; formal analysis, H.K., A.B. and E.V.; investigation, H.K.,
A.B. and E.V.; data curation, H.K., A.B. and E.V.; writing—original draft preparation, H.K.; writing—
review and editing, H.K., A.B. and E.V.; visualization, A.B.; supervision, A.B. and E.V.; project
administration, A.B. and E.V.; funding acquisition, A.B. and E.V. All authors have read and agreed to
the published version of the manuscript.
Funding: This research received no external funding.
Data Availability Statement: The data reported in the present study are available upon request;
please refer to the corresponding author when asking.
Conflicts of Interest: The authors declare no conflict of interest.
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nanomaterials

Nanomaterials 2022, 12, 2105. https://doi.org/10.3390/nano12122105 https://www.mdpi.com/journal/nanomaterials

and extensively use nanotechnology [5]. Thanks to the emergence of nanotechnology in

2. Materials and Methods

Table 1. Physicochemical Properties of Synthetic Ester, MIDEL 7131.

Property MIDEL 7131

Table 2. Characteristics of the nanoparticles.

NPs Fe3 O4 ZnO ZrO2 SiO2 Al2 O3 Al2 O3

2.2. Samples Preparation

Figure 1. The preparation procedure of nanofluids (NFs).

2.3. Stability of Nanofluids

Unstable NF Stable NF Highly Stable NF

Nanomaterials 2022, 12, 2105 6 of 25

For the comparison and quantification of PD activity, we are interested in the PD

Nanomaterials 2022, 12, 2105

Table 3. Zeta potential and electrical conductivity of nanofluids samples.

Mean AC BDV, SE/ZrO 2 Max/Min values

Mean AC BDV, SE/SiO2 Max/Min values

3.4.1. Statistical Analysis of AC Breakdown Voltage Outcomes for 2 mm Electrodes Gap

Nanomaterials 2022, 12, 2105 13 of 25

Data (SE) Data (SE)

Data (SE) Data (SE)

Data (SE) Data (SE)

Data (SE) Data (SE)

Normal fit curves.

Data (SE) Data (SE)

Data (ZrO 2, 0.1 g/L) Data (SE)

(0.1 g/L) Normal 77.40 11.04 81.90 8.62 87.30 5.94

(0.5 g/L) Normal 79.00

(0.4 g/L) Normal 83.00

(0.5 g/L) Normal 78.50

3.5. Partial Discharge Activity of Al22O O33and

Nanomaterials 2022, 12, 2105 21 of 25

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