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2004 lnrernarionul Co,ference on Solid Dielecrrics, Toulorcte, Fvance, Juh, 5-9, 2004

Electrical and Mechanical Strength of Mineral Filled Epoxy Insulators


in Correlation to Power Loss Factor

'

F. Gerdinand I*, M. Budde I, and M. Kurrat


I Technische Universitat Braunschweig,
Institut fur Hochspannungstechnik und Elektrische Energieanlagen,
Schleinitzstrasse 23,38106 Braunschweig, Germany
* E-mail : f.gerdinand@tu-bs.de
Abstract: Polymeric materials like mineral filled and
fibre reinforced epoxy resins were applicated in many
power apparatus for electric insulation. Compared to
ceramic and glass the composite insulators based on
mineral filled polymers have many advantages. Epoxies
offer new possibilities in developing electric insulations,
especially to reach more compact design in electric
power equipment. Due to their good adaptability, their
convenient manufacturing technology, their very good
electric and mechanical properties, mineral filled epoxies
are the preferred duromeric materials for many high
quality insulating systems. These materials for outdoor
and indoor use show ageing phenomena under
environmental stress which is not exactly known up to
now. For this reason it is important to get a reliable state
of estimation with loss factor and partial discharge
measurement. Mineral filled epoxy test specimens are
aged by water immersion due to environmental stresses
in outdoor applications. The loss factor, partial
discharges (PD), the glass transition temperature, the
electrical strength and mechanical properties are
measured in selected time intervals. The measuring
results and a theoretical explanation of ageing effects on
electric and dielectric parameters are presented.

INTERFACIAL AGEING PHENOMENA


MINERAL FILLED EPOXIES (MCEP)

IN

Polymeric composites are subjected to complex ageing


phenomena caused by physical and chemical reactions at
the large inner surfaces between filler and resin.
Degradation processes like partial discharges, moisture
attack or attack by SFs decomposition products are
strongly related to the state of adhesion in the
microscopic interface between filler and resin.
Delamination in this interface can lead to an accelerated
ageing and degradation of the most important material
parameters in an inadmissible way.

INTRODUCTION
Composite insulation consists of an organic polymeric
matrix, i. e. epoxy, which is filled or reinforced with
mineral powder, glass fibre or wollastonite. For
suspension or post-insulators in outdoor applications
crystalline quartz powder as a suitable filler is often used.
These composite materials have one thing in common - a
large internal microscopic interface between filler and
resin. This interface is the weakest part in composite
materials [3, 81. The quality of the material depends
evidently on the adhesion between filler and resin. A low
adhesion leads quickly to accelerated ageing processes
caused by moisture attack, partial discharges and
electro-mechanical forces. The loss factor measurement
and partial discharge analysis can help to classify
materials and can give more information about the
ageing state of materials. In opposite to breakdown
experiments, ,,dielectric diagnostic" methods are
non-destructive. Ageing effects can be measured several
times and changes can be monitored from the ,,new" to
the ,,aged state.

Fig. 1. Ageing effects in microscopic interfaces [8]


Partial discharges are driven by a high local electric field
strength and prefer to propagate along local weak spots.
The phenomena is well known as treeing [4]. The
weakest spots are arranged at the interface (incomplete
moistened areas, blisters, micro cracks: top left in Fig. 1)
so that partial discharges and treeing appear in or near the
interface. If the energy is high enough, the bonding
between filler and resin will be attacked and further
cracks with increasing PD intensity appear. This positive
feedback mechanism finishes in the interfacial
breakdown mechanism [SI resulting a total discharge and
destruction of the composite. Moisture induced ageing
destroys the adhesion between resin and filler as well as
the fillers stmcture itself by hydrolysis and corrosion.
This destruction (different crystallisation state,

delamination, damaged filler surfaces: Fig. I ) means an


internal loss of adhesion and can he detected by dielectric
measurements [SI.

The electric breakdown strength is also estimated with


the cone shaped test sample in Fig. 2. Due to high electric
strength and surface discharges, the test arrangement
according to IEC 60243 method is not applicable [8].

EXPERIMENTAL SETUP
Differential Scanning Calorimetry
Dielectric Parameters
For the measurement of the dielectric parameters E; and
tan&,IEC 60250 standardized method is applied with the
help of a transformer ratio arm bridge at a power
frequency voltage of 1000 V and a frequency of 50 Hz.
Disks of 70 mm diameter with a thickness of 3 mm and
discs with 46 mm diameter and a thickness of lmm and 2
mm are mounted in a guard ring electrode arrange-ment
~71.

Differential scanning calorimetry is a technique used to


determine what physically and chemically happens to
polymers when they are heated. Polymers have a higher
heat capacity above the glass transition temperature than
they have below it. This results in a step of ow plot
which occurs at the glass transition temperature [2].
Above the glass transition temperature polymers are
transformed into a rubber like state.
MEASURING RESULTS

Mechanical Parameters
The mechanical crack resistance is evaluated with the
"Double Torsion Test" (DTT). The DTT was developed
to test polymeric materials with support functions after a
first crack initiation. The required plate shaped samples
(dimensions 80 mm x 34 mm x4 mm) have a defined
notch (60 ", 1 mm depth) exactly in the middle of the
plate. For the execution of the DTT a pressureltension
machine standardized in DIN 51221 and a special
hearing support [I] is required. During the experiment,
the force F and the displacement s of the stamp are
recorded. The experiment is finished if the plate breaks
or if the force decreases down to 99 % of its maximum
value (F,nax).Fmx is estimated from the F(s) diagram in
accordance to [I].
Partial Discharge Measurement
Breakdown Strength Measurement

And

Electric

To get more knowledge of the degradation state and the


residual life of the used material, artificial ageing tests
are necessary. To force and to accelerate moisture
induced interfacial ageing phenomena the test specimen
are immersed in distilled water at 50OC [7,8]. The electric,
dielectric, mechanical material parameters and the glass
transition temperature (Fig. 3 - 8) are measured during
the ageing procedure at exactly defined time intervals [6].
In order to check the sensitivity of the measured
quantities to artificial ageing, a typical insulation system
for indoor applications is aged under outdoor conditions
in a first step. The following basic cycloaliphatic
carbonic acid hot curing formulation is used
Resin, Araldite 2, CY 184 (cycloaliphatic),
100 pt.
Hardener, HT907 (cycl., carbonic acid),
87 pt.
I pt. Accelerator, DY071,
282 pt.
Si02filler, W d ) .

According to IEC 60270 the PD tests were performed at


50 Hz alternating voltage. Therefor cone shaped test
samples (s = 1 mm) are used (Fig. 2). The maximum
electric field strength is concentrated in the epoxy at the
tip of the high-voltage electrode.

tans

days ofwafer immersion

Fig. 3. Permittivity and loss factor during water


immersion (sample thickness 1 mm)
grouiid elrcliode
(evopoiaicd \villi timiuinr

Fig. 2. Cone shaped test sample for the measurement of


partial discharges and electric breakdown strength
(Schwaiger's field coefficient q = 0.62)

Aralditc CY 184, HT907 and DY071 are products ofHuntsman AG,


Base!, Switzerland
'I

WIZ is a product of Quamuerke Frechcn GmbH, Frechen, Germany

tzo

100

80

60

;
I

40

20

0
0

11

10

day. otWa.r Im_./M

Fig. 4. Electric breakdown strength during water


immersion

<

J
4
day. otw*.r

7
i I i I * Z t , 5
imm.rrion

Fig. 5. Mechanical crack resistance during water


immersion

m
..
0

10

15
d..*W.b,

20
inm.ion

I
I
2s

!
I
Y)

15

Fig. 6. Glass transition temperature during water


immersion

DISCUSSION
The results of the experiments show that measured
quantities are sensitive to artificial ageing. In outdoor
applications hydrolysis by moisture attack appears. The
consequences are the loss of internal adhesion and an
increase in the conductivity. This is demonstrated by an
increase of the dielectric parameters (&, tan&) in Fig 3.
Simultaneously the electric breakdown strength, the
mechanical crack resistance and the glass transition
temperature decrease (Fig. 4 - 6). The measured electric
breakdown strength (Fig. 4, Fig. 9) is only the short time
strength, hut a local thermal breakdown cannot be
excluded. For a complete electric classification the
measurement of local thermal and partial discharge
breakdown is also needed.

50

120

im

240

300

*pi

360

Fig. 8. Accumulated apparent charge in dependance of


phase angle and days of water immersion
Fig. 7 shows an increasing apparent charge during water
immersion, fig. 8 presents the accumulated apparent
charge. Apparent charge magnitude and distribution
changes significantly at high electric stress. The aim of
all these investigations is the development of diagnostic
methods for classifying insulating materials. The
following criterions for our investigated test specimens
could be given:

If the dielectric loss factor rises after some days of


water immersion up to 2000.104, the investigated
composite insulating system shows degradation
effects.
The progressive increase of loss factor (500104)
indicates that the investigated material structure has
been degraded (fig. 3)
No negative effects can be detected before dielectric
loss factor reaches 50010" (fig. 9-10).
The influence on the mechanical properties is
inferior.
The significant decrease of the glass transition
temperature shows physical and chemical
destruction in the investigated material.
The accumulated apparent charge (fig. 8) shows an
increase ahout several orders of magnitude during
ageing.

and epoxy matrix and conductivity increase. The


decreasing glass transition temperature is an indicator for
these processes, which finally lead to a reduction of
mechanical crack resistance, electric breakdown strength
and a rise of PD activity. Due to the definite temporal
behaviour of the material properties a correlation
between loss factor and degraded properties is evident.
In a first attempt the loss factor measurements of plate
samples are correlated to the mechanical crack resistance,
electric breakdown strength and the glass transition
temperature. Obviously there is a limiting loss factor
value, which clearly i.ndicat$a a degradation of the
internal polymer structure. Dielectric diagnosis is thus a
good non-destructive tool to detect ageing phenomena.
The measurements on PD activity could assume a
possible correlation with dielectric results. Therefor a
couple of measurements will be added soon.

REFERENCES

iffin

5ffi

1500

2500

2000

tan 6 1107
. .

Fig. 9. Mechanical crack resistance and electric


break-down strength in dependence of loss factor
(sample thickness: 1 and 2mm)
;loPCl

'

105 ,

85
~

500

10W

1500

2000

2500

3000

3500

tan 6 [io?

Fig. IO. Glass transition temperature in dependence of


loss factor (sample thickness: Imm)

Ciba Geigy: "Double Torsion Test", Testing


Method NI. PM2 16-0189
Mettler
Toledo:
TA-Applikationssammlung,
Schwerzenbach, 1997, Schweiz
F. Gerdinand, M. Budde, M. Kurrat: State
estimation of mineral tilled epoxy insulators with
loss factor measurement, International Sympo-sium
of High Voltage Engeneering, Delft, 2003,
Netherlands
H. C. K h e r : Interfacial phenomena with
composite materials. International Conference on
non-ceramic insulators, Singapore, June, 1996
A. Kutil, K. Frohlich: Partial discharge phenomena
in composite insulation materials. 1995 Annual
Report of the Conference on Electrical Insulation
and Dielectric Phenomena, Virginia Beach, VA
USA, October 22-25, 1995
H. C. Kamer, M. leda: Technical aspects of
interfacial phenomena in solid insulating systems,
ICAPDM, Tokyo, 1991, Japan
H. C. Karner, W. Kodoll, J. M. Seifert, T. Tanaka,
and M. Nagao: Interfacial Phenomena affecting
electrical Insulating Properties in Composites,
CIGRE RRT, ELECTRA No. 202,2002.
J.
M.
Seifert:
Grenzflachenund
Verbundpro-bleme in mineralisch gefiillten
TU
Epoxidharz-formstoffen.
Dissertation,
Braunschweig, 1998

ACKNOWLEDGEMENTS
CONCLUSION
Water immersion in destilled water is a good artificial
accelerated ageing test for outdoor insulation. The
material properties of the investigated cycloaliphatic
carbonic acid hot curing formulation degrade during the
ageing process. The loss factor and the permittivity
drastically increase within some weeks by hydrolysis.
The subsequent loss of internal adhesion between filler

The authors would like to thank the DEUTSCHE


FORSCHUNGSGEMEINSCHAFT for their financial
support. They also wish to express their gratitude to the
Huntsman AG, Switzerland, and the Quarzwerke
Frechen GmbH, Germany, for their support.

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