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ABSTRACT
Changes in the dielectric breakdown field of polyimide (PI) films have been studied
from 25 to 400 °C under dc ramps. Both the area (from 0.0707 to 19.635 mm2) and
thickness (from 1.4 to 6.7 µm) dependences of the dielectric breakdown field have been
carried out using the Weibull distribution function. The 63%-breakdown field value
(i.e. the -scale parameter) of PI shows a decrease with increasing area, thickness and
temperature but always remains above 2 MV/cm. The -scale parameter of the
distribution shows a typical decrease with increasing area, however, it exhibits an
increase with increasing thickness. This ‘curious’ behavior is discussed on the basis of
the percolation theory. No temperature-dependence is clearly observed. Moreover,
physical interpretations are carried out using the pre-breakdown current analysis.
Index Terms — Polyimide (PI), dielectric breakdown, dielectric strength, area,
thickness, temperature, Weibull distribution.
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IEEE Transactions on Dielectrics and Electrical Insulation Vol. 17, No. 1; February 2010 19
distortion due to space charge, temperature increase due to low critical temperature (T<TC1) and is roughly not
local heating and thickness deformation due to Maxwell depending of the temperature despite in some cases below
stress [15, 16]. room temperature, a slight increase can be observed [16].
The temperature dependence of the dc dielectric The second one is the thermal breakdown process
breakdown field (EBR) of polymers usually shows a appearing for an intermediate temperature range
decreasing behavior with increasing temperature. However, (TC1<T<TC2). It is initiated by the steady state or impulse
this decrease appears as non-linear displaying different slopes thermal processes. Finally, above a high critical
in the EBR thermal dependence, as shown in Figure 1. temperature (T>TC2), an electromechanical mechanism is
preferred due to deformations and softening of polymers
(II) induced by the electrostatic forces between the test
(III)
electrodes.
Dielectric breakdown field EBR
(I)
Typical
experimental curve
2.2 STATE OF THE ART OF THE DIELECTRIC
BREAKDOWN FIELD OF POLYIMIDES
Few papers present a combined study (thickness,
electrode area and temperature) of the dielectric breakdown
field of PI. Table 1 shows a review of the dielectric
TC1 TC2 Temperature
breakdown field values of PI found in the literature,
varying with different experimental parameters [8–11, 17–
(I): T<TC1; Electronic avalanche breakdown 25]. A wide range of EBR values has been reported up to
(II): TC1<T<TC2; Thermal and electro-thermal breakdown now, usually between 1 and 5 MV/cm, but the influence of
(III): T>TC2; Electromechanical breakdown the different parameters is not clearly identified when
combined to another one particularly if extrapolation laws
Figure 1. Typical temperature dependence of the dielectric breakdown are under concerns. Last, a statistical approach of the
field of polymers and the failure processes related (after [15]). dielectric breakdown phenomenon is not always used to
provide accurate and comparable results. It, nevertheless,
Three breakdown processes are usually cited. The first constitutes the state of the art regarding the thickness, area
one is the electronic avalanche breakdown which is a pure and temperature dependence of the dielectric breakdown
electronic breakdown. This phenomenon occurs below a field of PI.
Table 1. State of the art of the dielectric breakdown field of PI varying with different experimental parameters.
Thickness (µm) Electrode area Temperature (°C) Voltage form EBR (MV/cm) Atmosphere Ref.
13 – 125 Ø 5 mm 25 ac (50 Hz): 500 V/s 3.1 – 4 transformer oil / dibutyl [19]
DC: 500 V/s 5 – 5.2 phthalate (DBP)
13 – 175 Ø 5 mm 25 ac: 500 V/s 0.8 – 3.75 transformer oil / DBP [20]
26 – 78 -196 – 300 dc: 0.5 – 10 kV/s 0.9 – 4.9 liquid N2, silicone oil [8]
Ø: diameter.
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20 S. Diaham et al.: Dielectric Breakdown of Polyimide Films: Area, Thickness and Temperature Dependence
Faraday cage
PI films have been obtained from a polyamic acid (PAA) K-type thermocouple
Temperature
plate in air. For higher film thicknesses, multilayer coatings (25-400 °C) control
-2
10 397
dE
3.2 MEASUREMENT SET-UP = 200 kV .cm −1 .s −1 ISC=20 mA
-3 dt
10
U (V)
I (A)
298
Dielectric breakdown field measurements have been -4
10
performed using a dc voltage ramp supplied by a 3.5 kV
198
FUG voltage source connected to the sample through a 10
-5
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IEEE Transactions on Dielectrics and Electrical Insulation Vol. 17, No. 1; February 2010 21
breakdown craters have rarely been observed near the failure F( )=63.2%, is the shape parameter. A high –
electrode edge (due to their neat circular design using value is related to a low scattering of the data. The location
microelectronic photolithographic masks, and also to the (or threshold) parameter has been set to zero.
small film thicknesses). In almost all cases, the final
location of the irreversible breakdown is near the center of (a)
the structure. A self-healing phenomenon has sometimes
Irreversible
been observed only within the largest area tested electrodes breakdown craters
(diameters Ø = 2.5 and 5 mm). In this case, few healed-
craters (~1 to 3) scattered within the metallization before
the irreversible breakdown were observed, as seen in Figure
5a. The self-healing craters within the metallization (in a Self-healing craters
poor quantity compared to other works [9]) are here
preferably related to a local extrinsic contamination during 2 mm
1 1
U BR
E BR = (1)
0,7
3 3
d 0,0
4
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22 S. Diaham et al.: Dielectric Breakdown of Polyimide Films: Area, Thickness and Temperature Dependence
The experimental data have been ranking using the the material bulk leading to the failure of the insulating
median rank approximation given by [29, 30]: layer. This behaviour has already been reported in organic
materials such as polypropylene [32, 33], aramid paper,
i − 0.3 polyester mylar and Kapton-H films [11], but also in liquids
F (i, n) = (3) [34, 35] and gases [36]. Last, it may be seen that the
n + 0.4 temperature has an effect on the Weibull parameter values
that will be discussed in section IV.3.
where i and n are the rank of a failed sample and the total
number of tested samples, respectively.
For plotting the Weibull distribution law, the Ø 0.3 mm
(a)
0
10 Ø 0.5 mm
transformation of equation (2) into equation (4) has been Ø 1 mm
realized: Ø 2.5 mm
Ø 5 mm
-2
j (A/cm )
10
2
⎡ ⎛ 1 ⎞⎤
log 10 ⎢log e ⎜⎜ ⎟⎟⎥ = β [log 10 ( x) − log 10 (α )] (4)
⎣ ⎝ 1 − F ( x) ⎠⎦
-4
10
Ø 0.3 mm
(b)
3.5 PRE-BREAKDOWN CURRENT-VOLTAGE Ø 0.5 mm
-1
CHARACTERISTICS 10 Ø 1 mm
Ø 2.5 mm
Figure 6 shows an example of the conduction current Ø 5 mm
j (A/cm )
2
4.1 ELECTRODE AREA EFFECT ON THE WEIBULL For the lowest breakdown fields (F(x)<10 %), it appears
PARAMETERS that PI displays a deviating behaviour of the distribution of
Figure 7 shows the cumulative probability of failure in PI the breakdown field values. Indeed, another slope of the
films both at room temperature and 300 °C versus the cumulative probability of failure with a lower value can be
dielectric breakdown field for the different electrode distinguished. Trying to fit a non-zero location parameter
diameters. The values of the dielectric breakdown field to the experimental data, a value close to the lowest
ranged from 0.6 to 7 MV/cm depending on the temperature dielectric breakdown field for each electrode area has been
and the electrode area. These orders of magnitude are in found.
agreement with those reported in [9] and [10] for equivalent For the study of polymers, a natural location parameter
PI film thickness ranges. could be the dielectric breakdown field of air (i.e. the
For each temperature, it is possible to observe that the minimum Paschen breakdown voltage ~300 V) due to the
cumulative probability curve shifts slightly towards lower presence of vacuoles in the film. However, the thickness
breakdown fields with increasing the electrode diameter. range investigated here is lower than the minimum vacuole
The scale parameter (F=63.2 %) decreases also with diameter allowing the occurrence of partial discharges (~8
increasing the electrode diameter. In the same way, the µm) and none of this kind of defects has been observed
shape parameter (i.e. the slope of the fitting straight line) even by microscopy. Otherwise, there is no obvious
decreases with increasing the electrode diameter. These two physical or technological reason to take into account a non-
simultaneous observations deal typically with an increase in zero location parameter. It appears more realistic to
the result scattering. They usually are characteristic of an consider that there is another Weibull distribution law for
increase in the probability to find defects or impurities in low electric fields (not investigated here) [14], more
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IEEE Transactions on Dielectrics and Electrical Insulation Vol. 17, No. 1; February 2010 23
pronounced with increasing the electrode area. A similar where kA and mA are empirical area coefficients. kA
discussion has been reported by Laihonen et al. on represents the extrapolated dielectric breakdown field for
polypropylene films [33]. The presence of two Weibull an area of 1 m2.
distribution laws across distinct field ranges could be due to
two failure mechanisms of different nature. The first one 7
occurring at low fields and more influent for large electrode 6
α (MV/cm)
appearing across the high field range could be explained by
3
a thermal and/or electromechanical origin.
2
25 °C
1
F (%) 200 °C
T=25 °C 300 °C
95.7
340 °C
400 °C (a)
log10[loge(1/1-F)]
0 63.2
1
27.1 0,01 0,1 1 10 100
2
Electrode area (mm )
-1 9.5
Ø 0.3 mm
Ø 0.5 mm 0.95
Ø 1 mm 25°C
-2 Ø 2.5 mm 200°C
Ø 5 mm
10 300°C
(a)
340°C
0,1 1 10 400°C
EBR (MV/cm)
1 β
F (%)
T=300 °C
95.7
(b)
log10[loge(1/1-F)]
0 63.2
1
27.1 0,01 0,1 1 10 100
2
Electrode area (mm )
-1 9.5
Ø 0.3 mm Figure 8. Changes in the scale (a) and shape (b) parameters versus the
Ø 0.5 mm 0.95
electrode area and for different temperatures (film thickness d=1.4 µm).
Ø 1 mm
-2 Ø 2.5 mm
Solid lines represent the best fits given by equation (6).
Ø 5 mm
(b)
Transformation of equation (5) into equation (6) allows
0,1 1 10
obtaining kA and mA fitting linearly data in Figure 8a:
EBR (MV/cm)
1
Figure 7. Cumulative probability of failure in PI films versus the
dielectric breakdown field at 25 °C (a) and 300 °C (b) and for different log 10 (α ) = log 10 ( k A ) − log 10 ( A) (6)
electrode diameters (film thickness d=1.4 µm). Solid lines represent the
mA
best fits given by equation (4) considering a confidence interval of 90%.
Table 2 lists the changes in kA and mA versus
temperature. These parameters allow extrapolating the –
Figure 8 shows the changes in the scale and shape parameter whatever the electrode area. It also appears that
parameters versus the electrode area for different the dielectric breakdown field of PI remains high (above 1
temperatures. Both the – and –parameters present a linear MV/cm) even for large areas and high temperatures.
decrease in a bi-logarithmic plot with increasing the
Table 2. Evolution of the kA and mA coefficients from equation (6) versus
electrode area. Assuming that the weak points present in the temperature for a PI film thickness of 1.4 µm.
material leading to a breakdown are randomly and Temperature (°C) kA (MV/cm) mA
uniformly scattered, it is known that the scale parameters
used to decrease with increasing the electrode area 25 2.33 18.64
following the area extrapolation law given by [31, 34, 36]: 200 2.02 20.92
300 1.88 24.06
1 340 1.14 15.05
−
α ( A) = k A A mA
(5) 400 0.61 9.87
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24 S. Diaham et al.: Dielectric Breakdown of Polyimide Films: Area, Thickness and Temperature Dependence
α (MV/cm)
Figure 9 shows the cumulative probability of failure in PI
versus the dielectric breakdown field for the different 2
thicknesses investigated. As expected, a unique Weibull
distribution law is observed.
300 °C
1 400 °C
F (%)
T=300 °C 1
95.7 1 2 3 4 5 6 7 8
Thickness (µm)
log10[loge(1/1-F)]
0 63.2
Figure 10. Changes in the scale parameter versus the PI film thickness
27.1 (electrode Ø 0.3 mm). Solid lines represent the best fits given by equation
(8).
-1 9.5
10
300 °C
by the thickness increase due to the increase in the 320 °C
probability to find defects or impurities in the bulk of the 340 °C
insulating layer leading to the failure. Such a behavior has 360 °C
380 °C
already been observed in PI films [8, 10, 19, 20]. Reporting 400 °C
the –parameter values in a plot versus the PI film 10
0
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IEEE Transactions on Dielectrics and Electrical Insulation Vol. 17, No. 1; February 2010 25
density required to form a breakdown path. It is evident that the dielectric breakdown field shows a slight decrease when
such a behavior may have a physical origin that cannot be the film thickness increases with values of the –parameter
resolved experimentally with the statistical accuracy even from 3.7 to 2.9 MV/cm and from 3.3 to 2.3 MV/cm,
with large experimental data, as seen in Figure 9. However, respectively at 300 and 400 °C.
the values obtained here from 8 to 30 are of the same order
and show the same tendency than those reported by 7
Laihonen et al on polypropylene films across the similar
thickness range [33]. Up to now, no clear interpretation has 6
α (MV/cm)
works have recently started in order to explain this
behavior. 4
3
Ø 0.3 mm
4.3 TEMPERATURE EFFECT ON THE WEIBULL 2 Ø 0.5 mm
Ø 1 mm
PARAMETERS 1 Ø 2.5 mm
As presented in section 2.1, the typical change in the Ø 5 mm
0
dielectric breakdown field of polymers usually decreases 0 50 100 150 200 250 300 350 400
with increasing temperature even if, in some cases below Temperature (°C)
room temperature, a slight increase can be observed [15, Figure 12. Changes in the scale parameter versus temperature for
16]. This decrease is usually due to thermal and/or different electrode diameters (film thickness d=1.4 µm).
electromechanical processes. In PI materials, the widest and
highest temperature region of investigation found in the
literature up to now has been reported by Nagao et al in Figure 13 shows the high temperature dependence of the
PMDA/ODA from -196 to 300 °C using a dc electric field –parameter versus geometrical changes. Contrary to the –
rising rate of 200 kV.cm-1.s-1 [8]. These authors observed a parameter, the –parameter is independent with increasing
slight increase in the dielectric breakdown field from -196 temperature.
to 25 °C, before measuring an exponential decrease up to
300 °C. A higher temperature range of investigation has 10
2
10
the whole temperature range of investigation, as shown in
[42]. The dielectric breakdown field of PI shows also a
behavior close to the one of the region II of the Figure 1, 1.4 µm
just between the two critical temperatures (TC1<T<TC2) and 3.6 µm
where TC2 often corresponds to the glass transition 6.7 µm (b)
0
temperature. So, a thermal origin of the breakdown process 10
300 320 340 360 380 400
is maybe supposed as the most probable failure mechanism.
PI films with various electrode areas have shown a Temperature (°C)
dielectric breakdown field from 4.3 to 6 MV/cm and from Figure 13. Changes in the shape parameter versus temperature for
1.9 to 3.3 MV/cm, respectively at 25 and 400 °C. For a different (a) electrode diameters (film thickness d=1.4 µm) and (b) PI
given electrode diameter of 0.3 mm (as seen in Figure 10), thicknesses (electrode diameter Ø = 0.3 mm).
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26 S. Diaham et al.: Dielectric Breakdown of Polyimide Films: Area, Thickness and Temperature Dependence
The only changes are induced by the geometrical [5] C. P. Wong, Polymers for Electronic and Photonic Applications,
London: Academic Press. Inc, 1993.
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[27] ASTM D149-97a, “Standard Test Method for Dielectric Breakdown Samir Zelmat was born in Sidi Bel Abbes,
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[30] C. Chauvet and C. Laurent, “Weibull Statistics in Short-term Professor at Paul Sabatier University, and the
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Breakdown Strength of Polypropylene Films: Area Dependence and Research Associate of the National Center of
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Insul., Vol. 8, pp. 248-252, 2001. Toulouse in 1999 as a Research Engineer. His
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Structure”, IEEE Trans. Electr. Insul., Vol. 26, pp. 1147-1152, 1991. their dielectric environnement. He is particularly
[39] J. H. Stathis, “Percolation Models for Gate Oxide Breakdown”, J. dealing with different high power and/or high
Appl. Phys., Vol. 86, pp. 5757-5766, 1999. voltage characterisation and diagnostic setups and methods.
[40] J. Suñé, “New Physics-Based Analytic Approach to the Thin-Oxide
Breakdown Statistics”, IEEE Electron Device Letters, Vol. 22, pp. Michaël Decup was born at Albi, France in 1982.
296-298, 2001. He received the M.Sc degree in electrical
[41] E. Y. Wu, J. Suñé, and W. Lai, “On the Weibull Shape Factor of engineering from Paul Sabatier Toulouse France
Intrinsic Breakdown of Dielectric Films and Its Accurate University in 2007. At present, he is working at
Experimental Determination—Part II: Experimental Results and the the Plasma and Energy Conversion Laboratory in
Effects of Stress Conditions”, IEEE Trans. Electron Devices, Vol. 49, order to obtain the Ph.D. degree in electrical
pp. 2141-2150, 2002. engineering. He belongs to the Dielectric
[42] S. Diaham, M. L. Locatelli, and T. Lebey, “High Temperature Materials and Energy Conversion team. His main
Dielectric Behavior of Al/Polyimide/Al Capacitor Structures”, IEEE research interest is to analyze the impact of
Vonf. Electr. Insul. Dielectr. Phenomena (CEIDP), pp. 97-100, 2006. fabrication and assembly technologies on the dielectric properties of
ceramic substrates used in power electronic applications.
Sombel Diaham was born in Montauban, France, Thierry Lebey (M’98) received the M.Sc. degree
in 1982. He received the M.Sc. and Ph.D. degrees in solid state physics in 1984, his Ph.D. in
in electrical engineering, respectively in 2005 and electrical engineering in 1989, both from
2007, both from the Paul Sabatier University of University Paul Sabatier in Toulouse. Since 1990,
Toulouse, France. In 2005, he joined the he is engaged with the French National Scientific
LAPLACE laboratory in Toulouse where he has Research Center (CNRS) where he is now Senior
been since 2008 an Associate-Professor. His Research Scientist. He is the author of more than
current research fields focus on the study of 60 journal and 100 conference papers and holds 8
dielectric materials for the insulating international patents.
environment (passivation and encapsulation) of high temperature and/or
high voltage wide band gap semiconductor power devices (SiC, GaN and
Diamond). His fields of interest cover from both the study of the physical
properties of insulating materials and their reliability in high temperature,
up to the study of their impact on the electrical characteristics of the
devices. He is co-author of 6 communications in international scientific
reviews and 8 papers in international conferences.
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