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2206 T. Tobias et al.

: Dielectric Breakdown Study of a Nanofluid Based On Goethite Nanoparticles

Dielectric Breakdown Study of a Nanofluid Based On


Goethite Nanoparticles
Tomas Tobias, Michal Rajnak, Peter Kopcansky and Milan Timko
Institute of Experimental Physics, Slovak Academy of Sciences
Watsonova 47
Kosice, 04001, Slovakia

Filippo Agresti and Simona Barison


Institute of Condensed Matter Chemistry and Technologies for Energy, National Research Council of Italy
Corso Stati Uniti 4
Padova, 35127, Italy

Bystrik Dolnik and Michal Rajnak


Faculty of Electrical Engineering and Informatics, Technical University of Kosice
Letna 9
Kosice, 04200, Slovakia

ABSTRACT
The study of electric breakdown in magnetic nanofluid is one of the basic
characterizations from the dielectric point of view. In this article we put effort to study
dielectric breakdown strength of the transformer oil doped with goethite rod-shape
nanoparticles. We use oscilloscope technique to catch the breakdown value for DC and
AC applied potential, respectively. The investigated sample was exposed to both, DC
and AC electric potential. We point out that for DC dielectric strength there is a
positive influence of goethite nanorods on dielectric strength till electrode gap doesn’t
exceed critical value. Otherwise, for AC electric potential there was practically no
effect on dielectric strength of the investigated nanofluid. In the result and discussion
we present more complex description of the measured data. We also provide
information about preparation processes of the fluid and detailed description of the
measurement setup.
Index Terms – magnetic nanofluid, breakdown, dielectric strength, transformer oil

1 INTRODUCTION transformer tank, especially around the winding and core,


which are the source of the heat and improves the cooling
IN the last decades, the dispersion of nanoparticles in
effect. Moreover, magnetic fluids can exhibit improved
transformer oils have shown promising thermal and dielectric
dielectric breakdown strength as compared to their carrier
properties which are making them attractive for use in the
liquid, what is quite paradox due to the fact that magnetic
power transformers as cooling and insulating media [1].
fluids contain solid nanoparticles. Recently, a novel theory
Cooling effectiveness enhancement due to the increased
explaining this paradox has been proposed in [6]. This theory
thermal conductivity by doping fluids with metallic
explains this fact in a way that nanoparticles act like free
nanoparticles was confirmed by several studies [2]. Masuda et
charge scavengers and this is in quite good agreement with
al [3] showed 32% and 11% increase in thermal conductivity,
experiments [7-9]. Electron scavenging performed by
respectively (Al2O3 and TiO2 with φ = 4.3 vol. %), Eastmann
conductive nanoparticles is a possible explanation of the
et al [4] showed 40% increase in thermal conductivity of
decrease in positive streamer velocity and consequently higher
nanofluid consisting of copper nanoparticles dispersed in
breakdown strength in magnetic nanofluids stressed by
ethylene glycol (φ = 0.3 vol. %). Furthermore, in the case of
positive voltage, as simulated in [10]. Electrons scavenging
magnetic nanofluids, the cooling improvement also stems
can be described as a conversion of free fast electrons
from the magnetic particles interaction with a gradient
developing a streamer by nanoparticles and changing them
magnetic field that a power transformer creates itself [5]. This
into negatively charged particles. It was found [10] that the
interaction can enhance the flow of insulating liquid inside a
relaxation time constant for magnetite spherical nanoparticles
Manuscript received on 28 February 2018, in final form 11 June 2018,
is much faster (τ = 7.47 x 10-14) than microseconds of streamer
accepted 12 June 2018. Corresponding author: T. Tobias. development. Positive streamer velocity is reduced by electron

DOI: 10.1109/TDEI.2018.007349
IEEE Transactions on Dielectrics and Electrical Insulation Vol. 25, No. 6; December 2018 2207

charging of the nanoparticles and the experimental results as viscosity (η = 7.6 mPa/s at 40 C ̊ ), oxidation stability with a
reported in [11] are important because a slower developing density ρ = 0.874 kg/dm3 at 20 C
̊ .
streamer can be extinguished faster. The similar approach has
been considered in other experimental works [12-14]. 2.1 GOETHITE AND NANOFLUID SYNTHESIS
Goethite is one of the most widely used iron oxides and one
A power transformer is one of the most important parts in
of the most widespread Fe oxides in the nature. It crystallizes
the electric power system network, it is a static device
usually along the a crystallographic direction [25].
consisting of a winding, or two or more coupled windings,
with or without a magnetic core. In electric power systems For the purposes of our experiments 100 ml of goethite
transfers power by electromagnetic induction between circuits nanorods suspension in the Nytro 10XN oil, stabilized with
at the same frequency, usually with changed values of voltage Sodium Docusate was prepared. The docusate was chosen
and current. [15]. There is no doubt, without reliable being a surfactant able to attach to the nanoparticles surface in
transformers, the growing demand for electricity cannot be water dispersion and then give a stable suspension in oil
satisfied. It is very important to assure transformers will be thanks to a good chemical compatibility between oil and
able to resist increasing demand for electricity without or docusate. The volume concentration of goethite nanorods was
minimum malfunctions [16-17]. Research results of many 0.01 %. The prepared suspension is quite stable for a couple of
researchers have shown dramatic improvement of insulating days so we needed to sonicate the suspension for 20 min
and thermal properties when nanoparticles are dispersed in before experiments performed.
transformer oil [1,18]. In the recent years, various types of A Goethite suspension into Nytro 10XN oil has been
nanoparticles have been used for the preparation of nanofluids obtained starting from a colloidal suspension of goethite
based on transformer oils. In the preparation process of nanorods into water. Goethite nanorods have been synthetized
nanofluids, researchers use non-conductive (i.e. Al2O3), semi- by a co-precipitation method using Fe(NO3)3 as a precursor
conductive (i.e. TiO2), conductive (i.e. Fe3O4) and many and NaOH as a precipitating agent and subsequent aging at
others nanoparticles to achieve the best results as can be seen room temperature for three days. A stable colloidal suspension
in the works [1,19-22]. From the above, one can consider has been obtained by purification of nanorods and subsequent
dielectric breakdown strength as an important transformer oil ultrasound irradiation into deionized water. The details of this
property. Breakdown voltage is voltage level that oil or preparation route are reported into a previous publication [26].
magnetic nanofluid is not anymore able to resist and discharge 0.086 wt% of sodium docusate (provided by Sigma-Aldrich)
occurs between electrodes [23]. has been dissolved into a 0.01 vol% (0.043 wt%) goethite
In this study we focus on the dielectric breakdown strength nanorods colloidal suspension in water. The suspension has
of Goethite nanofluid based on Nytro 10XN transformer oil been sonicated for 20 min at 40 °C into a sonication bath to
under both, DC and AC voltage applied. Goethite better disperse the nanorods and favor the adsorption of
nanoparticles were extensively studied in the last decades. sodium docusate on the surface of nanorods. The suspension
Investigations showed orientation ordering under the electric has been stirred twelve hours. The goethite nanorods have
field (the Kerr effect) [22]. If we take into account goethite been precipitated by centrifugation and dried at ambient
nanoparticle’s shape (nanorods) [24] and electron scavenging atmosphere at 105 °C for 1 h. An adequate amount of Nytro
by nanoparticles, consideration should be given to the 10XN oil has been added to the dry powder and sonicated into
influence of nanoparticles ordering under the electric field on a sonication bath at room temperature for 15 min to obtain 100
dielectric strength. In majority of the nanofluids, there are mL of a 0.01 vol% stable suspension. SEM (Scanning
spherical nanoparticles for which positive influence on Electron Microscopy) picture of goethite nanoparticles can be
dielectric strength was observed as mentioned above. We are seen in Figure 1.
interested if there is a shape influence on dielectric strength by
doping the transformer oil with goethite nanorods. Also there
is a parallel between relaxation time under the electric field
influence of spherical and rod shape nanoparticles what we
assume for oil with a low permittivity is the same. Result of
these assumptions is in free charge scavenging improvement
based on the idea that a longer particle can possibly
accumulates more free charge compared to a spherical shape
particle. We also provide suggestions for suitable breakdown
model to explain breakdown occurrence under the
environment conditions while measurements were performing.

2 PREPARATION OF THE NANOFLUID


The investigated nanofluid is based on transformer oil
Nytro 10XN. Manufacturer denotes it is suitable for power
and distribution transformers, has good heat transfer, low Figure 1.  SEM picture of goethite nanorods.
2208 T. Tobias et al.: Dielectric Breakdown Study of a Nanofluid Based On Goethite Nanoparticles

3 EXPERIMENTAL METHODS
3.1 INSTRUMENTATION
The experimental measurement of the breakdown voltage of
the oil was performed according to the scheme in Figure 2.
The distribution of the electric potential and electric field
strength E in the experimental setup was simulated by the
finite element method magnetics (FEMM 4.2) using the
triangular element mesh and the iterative conjugate gradient
solver. The resulted distribution is depicted in Figure 3 and
Figure 4. The measuring circuit consists of a function arbitrary
waveform generator Agilent 33220A (G), digital storage
oscilloscope Rigol DS 1102E (DSO), high-voltage power
amplifier Trek 40/15 (HVPA) and measuring vessel.
Figure 4. Distribution of the DC electric field strength E for Nytro
10XN oil and electrode distance of 2 mm just before the breakdown.
HV – High Voltage, GND – Ground.

voltage power amplifier is from 0 V to ±40 kV and the output


current is up to ±15 mA.
The measuring vessel is constructed of two pieces of
insulating material and two copper electrodes placed inside the
measuring vessel. One electrode is fixed on the wall of the
Figure 2. Breakdown voltage measurement circuit scheme.
measuring vessel, the second counter electrode is mounted on
a movable arm with a micrometer screw (MS). The copper
electrodes have a cylindrical shape. The copper electrode
diameter is 20 mm and the height is 5 mm. By moving the
copper electrode using the micrometer screw, the distance
between the copper electrodes can be set with 10 microns
accuracy.
3.2 EXPERIMENTAL PROCEDURE
To ensure a smooth increase in the test voltage, a periodic
sawtooth voltage waveform was applied. The increase of 200
V/s in test voltage was chosen in the experiment. To achieve
an increase in the test voltage of 200 V/s, it was necessary to
set the period T of the sawtooth voltage waveform to 200
seconds and the amplitude (peak to peak) of the sawtooth
voltage waveform set to 10 volts with 5 volts DC offset. The
output voltage from the function arbitrary waveform generator
was connected to the input of the high-voltage power amplifier
(IN) and simultaneously to the channel A of the digital storage
oscilloscope. Thus it was possible to monitor the time course
of the voltage in the input of the high-voltage power amplifier
at any time.
The breakdown voltage of the oil sample was determined
Figure 3. Distribution of the DC electric potential for Nytro 10XN oil
and electrode distance of 2 mm just before the breakdown. HV – High
from the time course of testing high-voltage waveform applied
Voltage, GND – Ground, MS – Micrometer Screw. to the electrodes. The high-voltage waveform applied to the
electrodes was measured with the digital storage oscilloscope
The function arbitrary waveform generator Agilent 33220A in the channel B by using of a precision voltage divider (DIV)
uses direct digital synthesis (DDS) techniques to create a with a dividing ratio of 1000:1. The breakdown voltage of the
stable, accurate output signal for clean, low distortion sine oil sample was measured at electrode distances of 0.25 mm,
waves, square waves and pulse, linear ramp, triangle, noise, 0.5 mm, 0.75 mm, 1 mm, 1.5 mm and 2 mm. Seven repeated
and DC waveforms. The digital storage oscilloscope Rigol DS measurements were performed for each electrode distance.
1102E has 2 channels with 8 Bit resolution and 100 MHz Each time course of the voltage applied to the electrodes,
bandwidth. All data in memory can be saved to a file using including the breakdown voltage, was saved to a xls file
USB or RS 232 interface. The gain of the high-voltage power format for further processing. The resulting breakdown
amplifier is fixed to 4000. The output voltage of the high- voltage was calculated as the arithmetic mean of the seven
IEEE Transactions on Dielectrics and Electrical Insulation Vol. 25, No. 6; December 2018 2209

values of the measured breakdown voltage for each distance.


Example of how the DC and AC breakdown is spotted on
oscilloscope is depicted in Figure 5a and 5b.

Figure 6. Dielectric strength measurement for oil Nytro10XN and


Goethite nanofluid under slow rising DC potential.

Figure 7. Dielectric strength measurement for oil Nytro10XN and


Figure 5. a) Example of how DC and b) AC breakdown is spotted on Goethite nanofluid under AC electric field.
oscilloscope (electrodes separation 2000 μm).

4 RESULTS AND DISCUSSION 4.1 DC DIELECTRIC STRENGTH ANALYSIS


We performed positive DC dielectric strength measurement.
Gained results of the investigated oil Nytro 10XN and In this case, we assume positive streamer formations in all
Goethite nanofluid based on that oil are interesting from electric field gradients applied. This case is more natural for
several points of view. First of all, it is very unusual behavior streamer development. Streamer propagates from low field
of the goethite nanofluid under the positive electric potential. region to the high field region. In this case, the source of
As can be seen in Figure 6 and Figure 7, there is an charge is the dielectric itself [23]. As can be seen in Figure 6,
intersection between pure oil and goethite nanofluid dielectric for the pure oil the bigger the distance between electrodes, the
strength dependence on the electrode separation distance. In higher positive voltage needs to be applied to initiate the
Figure 6 one can see the dielectric strength improvement until breakdown. Breakdown voltage increases moderately till
the electrode separation doesn’t exceed 1000 μm; there is a distance between electrodes is under 1 mm. Above 1 mm one
decrease in the DC dielectric strength for larger separations. can see steep inclination in breakdown voltage. Beside this,
On the other hand there is AC breakdown measurement. for smaller gaps between the electrodes, values of the
One can see in the Figure 7 there is opposite trend to DC breakdown voltage are not scattered as for larger gaps. The
breakdown. Till electrodes distance is lower than 1000 μm key factor to generate breakdown is the electric field intensity
Goethite nanoparticles have a decreasing effect on AC (Equation 1):
dielectric strength but for bigger distances than 1000 μm there
is an improvement in the AC dielectric strength. 𝐸 (1)
2210 T. Tobias et al.: Dielectric Breakdown Study of a Nanofluid Based On Goethite Nanoparticles

where V is the applied voltage and d electrode separation. AC dielectric strength by doping the oil with goethite
Logically, as mentioned previously, increasing d needs to nanorods. Despite this, in some cases it is known that doping
result in increase of V, also streamer development is longer for dielectric fluid with nanoparticles increases breakdown
bigger gap (potential increase step was 200 V/s). strength as reported for example in [11]. In our case it is hard
These results are quite logic but our focus is aimed to oil to find a suitable theory for AC breakdown strength but still,
doped with Goethite nanoparticles curve. Remarkable we can provide analysis. One can consider assumptions as
improvement in dielectric strength till 1000 μm separation reported in [10] but it is necessary to consider the impact of
between the electrodes (2 times bigger dielectric strength for goethite particles’ geometry in our case. Charge relaxation
oil doped with goethite nanoparticles) one can interpret as time constant for transformer oil/nanoparticle (spherical)
goethite nanoparticles play a role as electron traps since they system is:
are polarized in the electric field. Then, the electric field lines
are expected to terminate on the particles surfaces and lead the 𝜏 (2)
migrating free charge in the particle trap center. On the other
hand, the polarized particle assembly and formation of long where ϵ1 and σ1 in equation 2 are permittivity and conductivity
chains is not expected because of the low field gradient and of the transformer oil and ϵ2 and σ2 are permittivity and
the small space between the electrodes. The particles can conductivity of goethite nanoparticle.
therefore act as electron scavengers and one can assume,
based on the goethite nanoparticles’ shape, that there is strong Taking into account values for Nytro10XN transformer oil
trapping center at the particle tips with the strongest electric (ϵ1 = 2.05 and σ1 = 7.92∙10-12 S.m-1) and goethite nanorods (ϵ2
field intensity. If the electrode separation distance exceeds = 11.7 [27] and σ2 = 6.25∙10-6 S.m-1, determined as σ = ρ-1,
greater distances than 1000 μm there is a space for goethite where ρ2 = 16ꞏ106 Ωꞏcm [28]) one can determine relaxation
nanoparticles to form a chain-like structure. In this case, the time which yields the value 8.59∙10-5 s. From this result it is
formed structures are more homogeneous and the presence of possible to consider electron scavenging model in both DC
sharp particle tips and strong trapping potentials are reduced. and AC mode at 50 Hz, as the half period takes 10 ms and
Thus, the migrating charge (electron) can gain enough energy there is enough time for the effective particle polarization.
to ionize other molecules to form the streamer and initiate Rod shape nanoparticles theoretically can accumulate more
breakdown process. Based on the experimental results and free migrating charge than spherical shape nanoparticles.
analysis, the DC breakdown enhancement of the studied Bigger the charged particle, slower the motion towards the
nanofluid can find a potential application in industry, electrode what results in increased dielectric strength. From
especially in regard to the slow changes in the electric field the graph depicted in Figure 7 there is an agreement with this
typical for DC industrial applications (such as DC power theory only for bigger distances.
transmission, transient phenomena in electric networks), for Therefore, regarding the DC breakdown study, we found
better approximation we also analyze AC dielectric strength maximal improvement of about 50 % as compared to the pure
measurements bellow. oil breakdown value. For a comparison with another studies,
4.2 AC DIELECTRIC STRENGTH ANALYSIS Kudelcik et al [29] investigated DC breakdown strength of
Fe3O4 nanofluids with a different concentrations and found
To explain electric failure under actual service conditions,
increase in dielectric breakdown strength of about 11 % for
one is always interested in AC dielectric strength analysis.
concentration 0.2 %v. Tomco et al [30] investigated DC
Measurements were performed under slow rising AC electric
breakdown strength of transformer oil and corresponding
potential. Electrical breakdown under AC electric potential is
Fe3O4 nanofluids with different concetrations with a maximum
much more complex problem than under the same DC electric
improvement of about 20 % in dielectric breakdown strength
potential. Complexity of the AC breakdown is in the space
for particle concentration 0.0025 %v.
charge producing and its influence on the applied electric
field. In one half of the cycle the cathode can inject electrons For the AC breakdown strength we found maximum
into dielectric liquid and anode extract charge from the improvement of about 15 %. In the work [31] Rafiq et al
dielectric. In the second half of the cycle anode and cathode measured the AC breakdown strength of mineral oil and
are reversed, discharge of the injected charge depends on the corresponding Fe3O4 nanofluids with different concentrations
applied electric field and drift towards the electrode. This local of nanofluids (5 – 80 % w/v) with a maximum breakdown
electric field is much lower for discharge than it is for improvement of about 16 % at 40 %w/v concentration of the
injection so in result we have accumulating space charge in nanoparticles. Jin et al. [32] measured the AC breakdown
dielectric. Due to AC potential there is a free charge motion, strength of pure mineral oil and corresponding fullerene
so called electrodynamic effect that complicates breakdown nanofluids with concentrations of 0.05 % and 0.1 %. The
study [23]. improvement in AC breakdown voltage was 19 % for 0.05 %v
Before AC dielectric strength analysis it is necessary to take fullerene concentration and 34 % for 0.1 %v concentration as
into account standard deviation from which we can see both compared to oil.
lines are in a very little variation from each other (Figure 7). Thus, our results have shown comparable values of DC and
This fact points to a possible meaning that there is no effect on AC breakdown improvement.
IEEE Transactions on Dielectrics and Electrical Insulation Vol. 25, No. 6; December 2018 2211

5 CONCLUSIONS [12] J. Lee and W. Kim, “Experimental Study on the Dielectric Breakdown
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This work was supported by the Slovak Academy of [18] Y. Zhong, Y. Lv, C. Li, Y. Du, M. Chen, S. Zhang, Y. Zhou and L.
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