Breakdown Voltage and Gassing Tendency of

Synthetic Esters Based MgO Nanofluids

2019 IEEE 4th International Conference on Condition Assessment Techniques in Electrical Systems (CATCON) 978-1-7281-4331-6/20/$31.00 ©2020 IEEE 10.1109/CATCON47128.2019.CN0032

P. Thomas
Dielectric Materials Division
Central Power Research Institute
Bangalore, India
thomas@cpri.in

Abstract—Synthetic esters that are readily biodegradable
have attracted attention as an alternative to mineral oil for
transformer applications. Researchers have focused on the
development of nanofluids; especially synthetic esters based
nanofluids are being developed for the next generation
insulating fluids. In the current investigation, synthetic ester
based MgO nanofluids with various weight percent (0.001 to
0.005 wt %) of MgO nano particles were prepared under
ultrasonication. The effect of MgO nanoparticles on the AC
breakdown voltage (BDV), loss tangent, and gassing tendency of
synthetic esters were studied in detail. The synthetic ester based
MgO nanofluids, besides showing enhanced electric breakdown,
also shows improvement gassing tendency behavior. Positive
response on the gassing tendency was observed for the
nanofluids. The synthetic ester based MgO nanofluids can be
preferred as an alternative medium for power transformer
insulation with reduced size to the conventionally used
petroleum based mineral oil.
annealed at ~750 °C/3h in a muffle furnace to get phase pure
ceramics.
B. Preparation of Nanofluids
The synthetic ester oil used in this study was obtained from
M/s M&I Materials India Pvt. Ltd [12]. Series of nanofluids
were prepared by mixing MgO nanopowders at various
concentrations: 0, 0.001, 0.0025, 0.005 and 0.01 by weight
percent in synthetic ester. To achieve homogeneous sample
with less agglomeration, the samples were ultra-sonicated
using probe ultrasonicator with a frequency of 60 kHz, pulsed
for 20 seconds at intervals of 10 seconds sonics off. The cycle
was repeated for 30 min to obtain homogeneous samples with
less agglomeration. The nanofluids thus prepared were stable
up to 48 h and thereafter, the particles starts settling. The use
of surfactants/ stabilizer could help in preparing stable
nanofluids, which needs to be studied in detail.

Keywords—nanofluids, synthetic ester, MgO, BDV, thermal III. RESULTS AND DISCUSSION
conductivity The nanofluids were characterized for parameters like tan
delta, resistivity, AC breakdown voltage (BDV), viscosity,
I. INTRODUCTION and gassing tendency behavior, as per guidelines given in their
Mineral oil exhibits good dielectric strength, possesses respective ASTM/IEC standards.
low viscosity, and is very cheap. Mineral oil is a mixture of
hydrocarbons, broadly classified as paraffinic, naphthenic and A. X Ray Diffraction of Nano MgO powder
aromatic. Paraffinic molecules can be either straight chain or The powder XRD analyses was carried out in 2θ range of
branched [1-3]. It undergoes severe ageing due to the presence 10–90 degrees (Pananalytical, X-pert Pro) using Cu Kα
of contaminants, oxygen and moisture, resulting in radiation. Fig. 1 shows the XRD pattern obtained for MgO
deterioration of insulating properties [4]. To overcome these nano crystallites before and after annealing for about 750 °C.
drawbacks various nanofluids were developed by adding very It is clear that the samples after heat treatment at around 750
small quantities nanoceramics having conductive [5], semi °C/3h exhibited well defined single phase with cubic
conductive [6], magnetic [7], and dielectric [8-10] properties, symmetry (Fig. 1b). Bragg reflections are indexed on the basis
into the base fluid, and studied in detail. These nanofluids of space group, Fm-3m (225), Z=4 with cubic lattice
exhibited tremendous improvement in critical parameters parameter, and a ~0.4210(4) nm, matching with JCPDS card
compared to base fluids. To explore the possibility of
obtaining next generation of insulating nanofluids, MgO
nanoceramic, which is a semiconductor/insulator possessing
cubic crystal structure and has several potential applications
[11], was chosen in this work. The nanofluids thus prepared,
were evaluated for the critical parameters and studied in detail.
II. EXPERIMENTAL
A. Preparation of Nanoceramics
The MgO nano ceramics was prepared in house by
combustion synthesis method as reported in literature [11]. In
a typical preparation, the starting material, Mg(NO3)2·6H2O
was initially dissolved in deionized water. Hexamine
(C6H12N4), also dissolved in deionized water, was mixed with
the magnesium nitrate solution and stirred well. The resulting
solution was heated very slowly, and when the temperature of
about 190 °C was achieved, a combustion of the whole
mixture was observed. The flame generated a white powder Fig. 1. X-Ray diffraction pattern of as prepared MgO and heat treated
during and after the combustion subsided, which was further @700 °C.

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number [11]. The average crystallite size was calculated using
the Debye-Scherrer’s formula,
k .λ
D=
β cos θ ,
where D is the average crystallite size of the particle, λ the
wavelength of the electron beam, β the full width at half
maximum (FWHM) of the peak, and θ is the Bragg’s angle of
diffraction. The average crystallite size was measured to be 65
nm.
B. AC Breakdown Strength
Breakdown voltage was measured as per the guidelines
given in the IEC 60156. The results obtained are shown as bar
chart in Fig. 2. AC breakdown strength results indicated that
the BDV values enhanced linearly up to 0.005 wt % MgO in
ester oil, and thereafter it decreased. The improvement in the Fig. 3. Tan delta measured at 90 °C for the nanofluids.
breakdown voltage can be attributed to semiconducting nature
of the MgO nanoparticles, which produce many electron
shallower traps in nanofluids [13]. The higher amount of
shallow traps available in the nanofluids contributing to the
rapid charge dissipation, and hence result in the improvement
of breakdown performance [13]. In order to see further
improvement in the AC Breakdown Strength, the MgO
concentration was increased to 0.01 weight percents in
synthetic ester. As per the mechanism proposed [13],
increased concentration of MgO should lead to more electron
shallower traps in nanofluids, and consequently, breakdown
strength of the oil was expected to improve further. However,
AC Breakdown Strength decreased, implying that the
nanoparticles having higher surface area had the tendency to
agglomerate, leading to saturation at an optimum
concentration, and hence the reason for the decrease in the AC
Breakdown Strength [14].
C. Tan Delta & Resistivity Fig. 4. Volume resistivity measured at 27 and 90 °C for the nanofluids.
Loss tangent and permittivity were measured as per the
guidelines given in the ASTM D 924 standards, and volume the MgO content was increased in the base oil, whereas at 90
resistivity as per ASTM D 1169 standard. These °C, there was sudden increase in tan delta for the nanofluid
measurements were conducted both at 27 °C and 90 °C, as with 0.001 wt% MgO, and interestingly, the tan delta value
shown in Figs. 3 & 4 respectively. As expected, the room showed a decreasing trend up to 0.01 wt percent. The addition
temperature tan delta value of the base oil was observed to be of MgO nanoceramic decreases the tan delta value to some
around 0.0038, which increased to 0.012 when the extent, which is a very interesting phenomenon. The volume
measurement was done at 90 °C. Room temperature tan delta resistivity values measured both at 27 and 90 °C on the
value of nanofluids indicated a decrease in tan delta value as nanofluids are presented in Fig. 4. By the addition of 0.001
wt% MgO in base oil, a sudden decrease in resistivity value
was observed, followed by an increasing trend. Similar results
have been observed for other nanofluids as well [9-11]. The
results indicated that the overall reduction in resistivity values
are not very drastic, but only marginal, indicating the absence
of any adverse effect on performance of nanofluids as
insulating oil.
D. Gassing Tendency
Gassing tendency behavior of the nanofluids was carried
out as per IEC 60628/A and the results obtained are given in
Fig. 5. Gassing characteristics of nanofluids result in linear
increase up to 0.005 weight %, due to the occurrence of high
rate of ionization. An earlier study [15] showed that gas
evaluation depends on the chemical composition of the oil,
electric field stress, temperature and time. In this study,
influence of nanoparticles on gassing behavior was observed,
Fig. 2. Effect of MgO nanoparticles on breakdown voltage of synthetic and synthetic esters based nanofluids exhibited positive
ester. response as compared to that of base fluid.

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 Fig. 5. Gassing tendency behavior of synthetic ester based MgO
nanofluids.
E. Viscosity
Fig. 6 shows viscosity as a function of temperature
measured as per ASTM D 445 standard. Room temperature
viscosity measurements indicate that there is no variation in
viscosity up to 0.01 weight percent addition of MgO
nanoceramics in synthetic ester. However, viscosity as a
function of temperature showed that kinematic viscosity
decreased as the temperature increased. The base oil having a
viscosity of 49.5 c-St @ 27 °C, decreased to 10.3c-St @ 70
°C. Interestingly the nanofluids up to 0.01 weight percent of
MgO in synthetic esters do not alter the kinematic viscosity,
following the base oil trend. In our previous works [9-11], we
showed that addition of nanoceramic up to 0.01 weight
percent in insulating oil did not alter viscosity of nanofluids.
IV. CONCLUSIONS
MgO nanocrystallites (~65nm) were successfully prepared
by combustion technique. Synthetic ester based nanofluids
exhibit tremendous improvement in critical parameters.
Electric strength values increased as MgO nanoparticles
increased up to 0.005 weight percent in synthetic esters. The
nanofluids showed increased thermal conductivity and
positive response in gassing tendency, and are considered as
the next generation of insulating fluids for transformers.
ACKNOWLEDGMENT
The management of Central Power Research Institute is
acknowledged for the financial support (CPRI Project No.
IHRD/2015/TR/7/15122015).
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