19th IEEE International Conference on Dielectric Liquids (ICDL), Manchester, United Kingdom, 25 – 29 June, 2017

Electrical Characterization of Synthetic Ester Liquid

Over Wide Temperature Range (-60°C / 200°C)

J. Muslim1,2, R. Hanna1, O. Lesaint1, J. L. Reboud1, N. I. Sinisuka3

(1)
Univ. Grenoble Alpes, CNRS, Grenoble INP, G2Elab, F-38000 Grenoble, France
(2)
PLN Indonesia, Jakarta 1216, Indonesia
(3)
Institut Teknologi Bandung (ITB), Bandung 40132, Indonesia

Abstract—Dielectric properties of synthetic ester oil are characterize liquids in such conditions. One of the main
investigated in wide frequency range (10 mHz – 1 MHz) and outcomes of using dielectric liquids instead of gels is their low
temperature (-60°C – 200°C) ranges. The aim is to determine the kinematic viscosity, which may also contribute to the cooling
ability of liquid insulation, to be used as encapsulating materials of electronic devices.
for high temperature power electronics modules. As far as the
ester remains in liquid state (above approximately -16°C), a The studied liquid is a synthetic ester oil type (Midel
typical frequency spectrum of the dissipation factor tan δ with 7131TM) which has not yet been characterized above 150°C.
two parts is observed. At low frequency, dielectric losses (tan δ > The influence of temperature and frequency on typical
0.10) are due to ionic conduction, and at high frequency losses electrical properties (relative permittivity İ’, conductivity σ,
are mainly due to dipolar relaxation. When temperature is dissipation factor tan į) will be studied by dielectric
increased, losses increase at low frequency, and decrease at high spectroscopy and conductivity measurements.
frequency. Results show that the liquid conductivity increases by
more than 3 orders of magnitude between room temperature and
II. EXPERIMENTAL SET-UP AND LIQUID USED
200°C. A slight decrease of permittivity is also observed,
correlated to the lowering of density at high temperature. This
behavior totally changes when the ester becomes a gel at low A. Experimental Set-Up
temperature. Dielectric relaxations reminiscent of solid materials Dielectric measurements in liquid are carried out by using a
then appear. test cell made up of two stainless steel coaxial electrodes set
within a faraday cage (Fig. 1). The electrode gap is 3.75 mm
Keywords—synthetic ester; relative permittivity, conductivity, and the air capacitance of the test cell is 22.5 pF. The test cell
tan (į), ionic conduction. is placed within a regulated climatic chamber, allowing the
control of temperature between -60°C and 200°C.
I. INTRODUCTION
High temperature power electronics has become possible
with the development of wide band-gap semiconductor
materials, such as Silicon Carbide (SiC) and Gallium Nitride
(GaN). Such materials could be used over 500°C in practice [1-
3], and up to 1000°C theoretically [4, 5]. Since these materials
also allow building high voltage semiconductors (exceeding 10
kV) of small sizes, one faces a very difficult problem of
electrical insulation, with both high temperatures and high
fields present simultaneously. To take full advantages of these
types of devices, packaging materials compatible with high
temperature are thus required. The technology todays enable
packaging elements such as ceramic substrates, brazing and
wire bonding, and passivation to be operated up to 600°C, Fig. 1. Schematic view of the test cell used for dielectric spectroscopy and
300°C and 250°C respectively [1]. However, the operating conduction measurements
range of silicone gels, commonly used as encapsulation
materials for classical power modules, is below 200°C. Dielectric spectroscopy measurements were carried out
Identification and characterization of new substitution using a broadband impedance spectrometer (Novocontrol
materials for encapsulation under higher temperature range is Alpha-A) within the frequency range from 10 mHz to 1 MHz.
therefore mandatory. The aim of this paper is to check the Dielectric properties such as İ’, tan į and AC conductivity
ability of dielectric ester to be used as an encapsulating (ıAC) are calculated from the impedance measurement under an
material at temperatures approaching 200°C. In addition, since alternative sinusoidal applied voltage of 1Vrms.
power electronics modules can also be used at very low Direct measurements of conductivity (ıDC) were also
temperatures (for instance in aircrafts), it is also interesting to performed according to advantage the IEC 61620 standard,

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 19th IEEE International Conference on Dielectric Liquids (ICDL), Manchester, United Kingdom, 25 – 29 June, 2017
using high sensitivity resistivity meter IRLAB LDTRP-2. This
system generates a ±10 V square wave, measures the charging
and conduction currents of the test cell, and displays its
capacitance (C) and conductance (G). The measured values of
C and G are in the ranges 10-10 – 10-15 S and 10 – 1000 pF
respectively. This additional measurement of conductivity ıDC
is then compared to conductivity values derived from dielectric
spectroscopy, in order to cross-check and validate the results.
B. Liquid used
Based on literature [6-8], Colza oils and more generally
natural ester liquids exhibit electrical properties degradation for
temperatures in excess of 120°C, with a rapid acceleration of
thermal aging processes. In this experimental study, a synthetic
ester oil (Midel 7131TM) was chosen regarding its advantages:
high fire point (316°C), low pour point (-60°C),
biodegradability and high moisture tolerance. Esters can absorb
greater amounts of water compared to mineral and silicone oils
without compromising their dielectric properties. Synthetic
esters provide good insulation properties and are widely used
in medium voltage transformers. However, despite their flash
point (260°C) and fire point (316°C) are quite high, the
maximum temperature in measurements was limited to 200°C,
in order to avoid the rapid chemical degradation that would
occur at higher temperature. Experiments were carried out in
ambient air. The total duration of measurements with a sample
was limited to a few hours, in order to minimize the influence
of oil ageing at high temperature
III. EXPERIMENTAL RESULTS
A. Permittivity measurements
The relative permittivity İ’ as a function of frequency,
depicted in Fig. 2 , shows that İ’ remains fairly constant in the
frequency range between 1 Hz – 100 Hz, and decreases when
temperature is raised. Below and above this frequency range,
different behaviors are observed.
Fig. 2. Variation of relative permittivity with frequency at different
temperatures
At low temperatures (< -16°C) and above 100 Hz a
decrement of permittivity is observed after a critical frequency.
The lower the temperature, the lower the critical frequency.
This behavior is correlated to the fact that in this temperature
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range, the ester is not any more a liquid, and starts to become a
gel. At the minimum temperature (-62°C), it gets the
appearance closely to solid.
Conversely, below 1 Hz and at high temperature (>50°C) a
large increase of permittivity is recorded. At low frequency
(e.g. 0.1 Hz), İ’ goes through a minimum when temperature is
increased (İ’ is minimum at 100°C at this frequency).
The decrease of permittivity versus temperature observed
over a large frequency range is to be correlated to the decrease
of liquid density. Fig. 3 shows the measured relative
permittivity obtained from dielectric spectroscopy at various
frequencies, compared to that calculated from capacitance
measurements with the resistivity-meter (IRLAB), and plotted
together with the liquid density (dashed red line). The liquid
density was obtained from the Midel 7131 datasheet between -
30°C to 140°C, and extrapolated to low and high temperatures
considering a linear trend. Previous papers reported variations
of permittivity in hydrocarbon liquids versus density, when
either pressure or temperature is changed [9]. Although the
relative variations of permittivity and density are quite similar
in our measurements, a more refined analysis [10] shows that
the density variations induced by the temperature cannot
entirely explain the observed permittivity variations.
Fig. 3. Relative permittivity and density as function of temperature
B. Losses and conductivity
Fig. 4 shows the typical behavior of dissipation factor tan į
versus frequency. On this plot, the black line indicates the limit
of measurement capabilities of the experimental system. Over a
large frequency range (1 Hz – 100 kHz), minimum tan į
measurements are limited to about 3.0×10-5. Between 100 kHz
and 1.0 MHz, the limit increases to about 10-3. In this range, all
measurements carried out above 100°C become similar and
identical to the system limit. Therefore, these measurements
are not valid. In a similar way, measurements carried out at
temperatures lower than -35°C and frequency below 2.0×10-1
Hz are erratic, and out of the system the measurement
capability.
When the ester is in liquid state (i.e. for temperature above -
35°C), a variation proportional to 1/f is observed at low
frequency (f). This variation is typical for losses due to
conductivity, according to equation (1), where σ DC is the dc
conductivity.
 19th IEEE International Conference on Dielectric Liquids (ICDL), Manchester, United Kingdom, 25 – 29 June, 2017

σ DC (1)
tan(δ ) =
2πf ⋅ ε S

At high frequency range, tan į is nearly proportional to f,

according to the relation (2):

ε∞ (2)
tan(δ ) ≅ (1 − )2πf ⋅τ
εS

where ε S and ε ∞ are static and optical permittivity, and IJ the

dipole relaxation time (which depends on the liquid viscosity
and thus on temperature). Consequently, the plot of losses
versus frequency gets a “V” shape, typical for liquids. At many
temperatures, the minimum values of losses are below the
measurement limit of the dielectric spectrometer (about 3.0×
10-5). When temperature is increased, the losses increase at low Fig. 5. Variation of AC conductivity (calculated from dielectric
frequency and decrease at high frequency. spectroscopy) with frequency

Fig. 6 shows that the dc conductivity deduced from Fig. 5, and

measured by the IRLAB resistivity-meter presents a good
agreement. σ DC increases by more than 3 orders of magnitude
between room temperature and 200°C.

Fig. 4. Tan (į) measurement as function of frequency

The evolution of AC conductivity versus frequency
deduced from spectroscopy measurements is depicted in Fig. 5.
It is obvious that when the ester is liquid (above -16°C), the
conductivity is frequency independent over a large frequency
range, from the lowest frequency investigated (10 mHz) up to a
maximum frequency that increases when temperature is raised.
Stable value of σ AC corresponds to the DC conductivity
( σ DC ), which strongly increases with temperature. The
relation between AC and DC conduction is expressed by:
σ AC ' = σ DC + k ⋅ 2πf a
where σ ' is the real part of σ AC , k is temperature-dependent
parameter, and a is the exponent of the power law.
For high frequency and temperature above -35°C, a nearly
linear variation of σ AC versus f with a slope close to 1 is
observed.
Fig. 6. Conductivity (deduced from the plateau of ıAC at 1 Hz and measured
by IRLAB) and inverse of viscosity as function of temperature
IV. ANALYSIS OF RESULTS AND DISCUSSION
Temperature has a large influence on the liquid density and
viscosity, and thus on its electrical properties. It is known that
in non-polar liquids such as esters, the conduction properties
are related to the density of ions, and to their mobility.
According to the Walden’s law, temperature has a direct
influence on ion mobility μ, since the latter is inversely
proportional to the viscosity Ș. Fig. 6 shows that both dc
conductivity and the inverse of viscosity Ș show a large
increase with temperature (T). However, the variation of ı (T)
(3) is higher than that of 1/Ș (T). Within the range from -30°C to
200 °C ı increases by nearly 6 orders of magnitude, while 1/Ș
is increased by only 3 orders. This indicates that the increase in
ion mobility cannot explain alone the recorded increase in
conductivity. Since that conductivity is proportional to the
product μn (with n is density of ions), and the mobility μ is
inversely proportional to the viscosity, then the ion density n
should be proportional to the product ı x Ș.

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 19th IEEE International Conference on Dielectric Liquids (ICDL), Manchester, United Kingdom, 25 – 29 June, 2017
Fig. 7 shows the Arrhenius plot for the product ı x Ș,
versus temperature from -26°C to 205°C. This plot shows that
the influence of temperature on conductivity is also due to a
large increase of the ion density when temperature is raised.
Fig. 7. Arrhenius Plot for product of conductivity and viscosity as function
of temperature
In non-polar liquids at very low fields, ions mainly result
from dissociation – recombination equilibrium of impurities,
characterized by a dissociation rate that increases with
temperature. Fig. 7 shows that the ion density fairly well
follows an Arrhenius-type variation, with a 0.217 eV activation
energy.
Fig. 8. Tan(į) at different high frequency and Ș/T as function of
temperature
As concerns the losses at high frequency, they can be
attributed to a dipolar relaxation mechanism. With such
mechanism and according to relation (2), tan δ is proportional
to the product of τ and 2ʌf . Since the dipole relaxation time τ
depends on temperature and is proportional to η/T [11], the
increase of tan δ versus temperature should compare with that
of η/T at fixed frequency. Fig. 8 shows a fairly good agreement
at two different frequencies. The temperature range was limited
to 100 °C, since tan δ measurements at high frequencies are not
valid at higher temperature.
At high temperature (> 150 °C) and very low frequency
(< 0.1 Hz), a relaxation phenomenon is also observed, probably
attributable to an electrode polarization process.
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V. CONCLUSION
The synthetic ester Midel 7131 exhibits at high temperature
up to 200°C a stable relative permittivity, over a wide range of
frequency (1 Hz and 1 MHz). Its conductivity increases by
more than 3 orders of magnitude between room temperature
and 200°C. At low frequency and high temperature, losses are
rather high (>1.0 at 50 Hz), mainly due to an enhanced ionic
conduction. The latter rapidly increases with temperature.
Conversely, losses at high frequency are attributable to a
dipolar relaxation process, and show a decrease when
temperature is raised. Further work (i.e. partial discharge and
breakdown measurements) is required to fully assess the
suitability of liquids for the insulation of high temperature
semiconductor devices.
ACKNOWLEDGMENT
Indonesia Endowment Fund for Education (LPDP) is
acknowledged for their financial support for first author.
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