Water Immersion/Liquid Permeation Resistance
Analysis of Micro/Nano-SiO2 filled Silicone
Rubber and Epoxy Composites for High Voltage
Insulation Applications
Hidayatullah Khan1, 2*, Muhammad Amin3, Ayaz Ahmad2, Muhammad Yasin1, 4
*1
Center of Excellence in Science and Applied Technologies (CESAT), Islamabad, Pakistan
2
Department of Electrical Engineering, COMSATS Wah Campus, Wah Cant, Pakistan
3
Electrical Engineering Department, GIK Institute of Engineering Science and Technology, Swabi, Pakistan
4
National University of Science and Technologies (NUST), Islamabad, Pakistan
E-mail:{hidayat.msk@gmail.com, prof_amin01@yahoo.com, ayaz.uet@gmail.com, m.yasin@seecs.edu.pk}
Abstract: In recent years, compared to the porcelain and glass
insulators, the silicone rubber (SiR) and epoxy based polymer
composite insulators have been widely investigated for high
voltage (HV) insulations, due to its promising electrical,
physical, and chemical properties. Multiple environmental
entities such as humidity, ultraviolet (UV) radiation, aqueous
solutions/moisture, micro-organisms, natural contaminations
etc., generally degrade the long-term performance of polymer
insulants. In the scope of this work, we have studied the
influence of micro and nano sized silica (SiO2) fillers on water
immersion/permeation resistance of room temperature
vulcanized silicon rubber (RTV-SiR) and epoxy composites.
Both RTV-SiR and epoxy based composite samples with
varying concentration of SiO2 particles were developed by
following the standard procedure (ASTM-D1418-10a). In order
to investigate the comparative immersion/permeation resistance
of SiR and epoxy blends, the 24h immersion tests and 02h
boiling water immersion tests were performed using ASTM-
D570 standard procedure. Results of 24h immersion tests
indicated that micro-SiO2 blend with epoxy (15%μSiO2 +
epoxy) showed comparatively higher immersion resistance i.e.
minimum mass uptake of ~10mg (0.092%). The 02h boiling
water tests revealed that neat epoxy samples loosed its mass of
~110 mg (-1.14%). The immersion/permeation reports suggest
that the liquid permeation and immersion resistance of polymer
blends is governed by particle size, type, and weight percent
(wt. %).
Key Words: SiO2, SiR, Epoxy, Water Immersion Resistance.
I. INTRODUCTION
Due to lighter weight, lower price, easy maintenance,
excellent electrical, thermal and anti-pollution flashover
performance, polymer composite insulators have been
widely used for high voltage (HV) insulations [1, 2].
However, insulants made of RTV-SiR and epoxy suffer
from various kinds of electrical, thermal and
environmental stresses [3]. Multiple factors such as
electrical discharge, ultraviolet (UV) radiation, natural
contaminations, gases, moisture/water ingress and high
temperature etc., affect the long-term performance of
polymer dielectrics [4-8].
Among these stresses, the penetration of liquids/moisture
plays a significant role in degradation of SiR and epoxy
insulators [9, 10]. Furthermore, due to partial-pressure
difference among environmental-conditions and dielectric
material structures, these factors (aqueous solutions) can
diffuse into insulator sheds which degrade both
‹,(((
mechanical and electrical characteristics of SiR dielectrics
through siloxane-chains hydrolysis and increase in loss-
tangent[11, 12]. Thus the water/liquid permeation into
polymer insulants is a serious dilemma for applications
where dielectrics are in direct contact with environmental
and electrical stresses. Therefore, in service conditions the
in-depth and quantified analysis of resistance to water
immersion/liquid permeation of RTV-SiR and epoxy is
needed [2, 13, 14].
For HV insulations, to enhance the immersion/penetration
resistance of SiR and epoxy insulants micro/nano-sized
particles (fillers) with optimum weight percent (wt. %),
are amalgamated with polymer matrix [10, 15-18]. The
filler particles make up a barrier to liquid/moisture
ingress, by extending the service life of polymer insulants
[17, 19, 20]. Thus variations in material characteristics are
governed by particle (filler) size, type, structure,
orientation, wt.% and dispersion in base matrix [21].
In the past many scholars have investigated the influence
of filler particles on liquids penetration/ingress resistance
of polymer insulants. Geo.Y et al.[12] investigated the
impact of solution concentration and solution type on
HTV-SiR with different ATH contents. They found that at
higher temperature, the SiR with lower alumina-tri-
hydrate (ATH) percentage absorbed less liquids compared
to higher ATH contents. Wang et al.[22], reported the
influence of aluminum-hydroxide and fumed-silica on
permeation and absorption properties of HTV-SiR. They
concluded, that the material internal free-volume have
significant role on liquids absorption. Furthermore, it is
investigated that water,moisture and fluids can penetrate
into weather-sheds and sheath of polymer insulator,
thereby causing fillers decomposition, interface
breakdown between polymer matrix and micro/nano-
particles, increase in leakage current and decrease in
dielectric strength [23, 24]. Hashiguchi et al.[25], studied
the impact of ATH on diffusion of water into SiR.
In other study Stevulova et al. [26] studied the water
absorption/penetration resistance of hemp-hurds and
inorganic-binder composites by performing the short-term
and long-term immersion tests. Wu et al. [2], investigated
the influence of surface modified ATH on electrical and
fluid penetration performance of SiR composites. In
addition, Ali et al.[27] examined the correlation among
SiR sample weight (immersed in water) with temperature
and particles loading. In other work Chow et al.[28],
reported that blending of glass-fiber/organo-

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montmorillonite with epoxy reduces water-uptake. Table 2. Blends chemical composition
Furthermore, the authors of [29], investigated the water
absorption behavior of wood-flour and polypropylene Inorganic Particles
composites. In our previous study [30], we have reported Sample Base
Details
the influence of micro/nano-silica on tracking/erosion code matrix
Type size wt%
resistance of SiR composites.
This novel work aims to analyze and compare the SR0 Neat SiR RTV-SiR - - -
influence of micro/nano-SiO2 on water immersion/liquid
permeation resistance behavior of SiR and epoxy 15%μSiO2
SRm RTV-SiR SiO2 3μm 15
composites. Furthermore, to quantify and compare, the +SiR
mass-uptake by SiR and epoxy blends, the 24h immersion 5%nSiO2
and 02h boiling water immersion experiments is SRn RTV-SiR SiO2 10nm 5
+SiR
conducted according to ASTM-D570 standard [31].
Neat-
EP0 Epoxy - - -
Epoxy
II. EXPERIMENTAL DETAILS 15%μSiO2
EPm Epoxy SiO2 3μm 15
+Epoxy
a. Materials and Samples Preparation
5%nSiO2+
In this work, the base materials such as low viscosity SiR EPn Epoxy SiO2 10nm 5
Epoxy
(RTV-615) and epoxy (diglycidyl-ether-bisphenol-A:
DER-331) were purchased from Wacker-Chemie
(Germany) and Dow-Chemical Beijing (China),
respectively. The micro and nano sized SiO2 particles
(fillers) were used in actual form as received from the
manufacturer. The principle features of SiO2 are
summarized in Table 1. The chemical composition of
SiR, epoxy and SiO2 can be seen from Figure 1(a, b, c).
Development of SiR and epoxy blends with micro/nano-
SiO2 particles were carried out in a high mow mixer
(HSM-100LSK) according to standard (ASTM-D1418-
10a) procedure [32]. SiR and epoxy blends stepwise
fabrication procedure and formulations are shown in
Figure 2 and Table 2, respectively. Additional, details
about sample preparation can be seen from our previous
work [30]. The developed blends of SiR and epoxy are
presented in Figure 3.

Table 1. Silica particles characteristics

Filler Particle size Density Supplier

Micro-
3μm 0.65g/cm3 US-Silica
SiO2
Nano-
10nm 2.23 g/cm3 Sigma-Aldrich
SiO2

Fig.1. Chemical structure of (a) Silicone rubber, (b) Epoxy, (c)

Silica

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Fig.2. Preparation procedure silicone rubber/epoxy blends
Fig.3. Developed blends of, (A) Silicone rubber and (B) Epoxy
b. Experimental setup for Water-Immersion/liquid
Permeation Resistance Analysis
In order to investigate the influence of micro/nano-silica
on vulnerability to water, moisture and liquids of SiR and
epoxy composites, the 24h immersion (at 25ºC) and 02h
boiling water immersion tests are sequentially performed
using the standard procedure (ASTM-D570) [33]. Figure
4, shows experimental setup for water immersion
resistance analysis of SiR and epoxy blends. Initially, all
samples were cleaned with distilled water and dried in
desiccators for one week at room temperature. Then
initial weight was recorded using notebook series (China,
.01g) digital scale. The samples were then placed in de-
ionized water for 24h at 25 oC (Figure.4a). After 24 h all
specimens were dried and re-weighted.
In addition, following the same standard (ASTM-D570)
method, the 02h boiling water immersion test (Figure.4b)
was conducted and the percent mass-uptake (water
permeation) of all samples was measured by using the
following equation:
− (1)
( )=
Where M (t), wt and wo stand for percentage absorption,
sample mass after immersion and mass before immersion,
respectively.
Fig.4. Water immersion/liquid permeation test setup
III. RESULTS AND DISCUSSION
A. 24 h immersion results of SiR and epoxy composites
For HV insulation applications, the moisture and water
absorbability of polymer insulants is one of the
significant parameters, which affect their thermal,
electrical and mechanical properties. Figure 5, shows
water absorbability (mass uptake/mg) and percent mass
gained of SiO2 reinforced SiR and epoxy composites after
24 immersion in distilled water. It can be seen that
compared to micro silica filled SiR (SRm) and epoxy
(EPm) samples, the neat (SR0, EP0) and nano-SiO2 (SRn,
EPn) samples showed higher mass uptake(less resistance).
This mass gain was 0.226% for SR0, 0.1813% for SRm,
0.19% for SRn, 0.32% for EP0, 0.092% for EPmand 1.25%
for EPn.The authors of [34], also observed the dissimilar

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absorption resistance for HTV-SiR blends with
hydrophilic fillers. They reported mass gain for HTV-SiR
composites immersed in varying concentrations of
glucose solutions.
Compared to all investigated samples of SiR and epoxy,
the only epoxy/micro-SiO2 blend (EPm) showed higher
immersion resistance (10 mg i.e. 0.092% mass-uptake),
whereas the epoxy/nano-SiO2 blend (EPn) indicated
maximum mass uptake (80 mg). This variation in mass
gain is attributed due to pre-existing voids, stronger Van
der Waal’s forces and lower free volume in polymer
matrix. Moreover, another reason of mass-uptake by
polymer blends is that water molecules may occupy the
free volume and pre-existing voids and thereby
weakening its thermal and electrical performance through
increased permittivity, conductivity and loss tangent [34].
Hence, it can be inferred that the micro-SiO2 filled epoxy
composites showed improved performance than SiR
composites after 24 h immersion (Fig.5).
Fig.5. 24 h water immersion results of SiR and Epoxy composites
B. 02 h boiling water immersion results of SiR and
epoxy composites
In order to examine the influence of temperature on liquid
permeation/immersion behavior of SiR and epoxy
composites, the 02 h-boiling water test was conducted at
100ºC. Figure 6, shows water-uptake (mass gain) of
SiR/SiO2 and epoxy/SiO2 micro/nano-composites. As
presented in the figure, RTV-SiR filled with micro/nano-
SiO2 absorbed less water than micro/nano-SiO2 filled
epoxy specimens. After 02 h boiling, the change in mass
uptake was 0.0045% for SR0, 0.181% for SRm, 0.48% for
SRn, -1.14% for EP0, 1.83% for EPm and 1.7% for
EPnsamples.
It can be seen that the resistance to water/liquid
ingress of SiR and epoxy blends was varied with
temperature as well as SiO2 particles concentration.
Among all investigated blends of SiR and epoxy, the
minimum mass uptake was noticed for neat SR0 (01 mg),
whereas higher mass-gain of ~200mg was noted for
micro-SiO2 filled epoxy composites.
In addition, over increase in temperature the only neat
epoxy blends (EP0) exhibited higher mass loss of ~110
mg instead of mass gain. It may be due diffusion of low
molecular weight (LMW) components from the material
bulk into the liquid (water) due to the LMWs
concentration difference [27, 35]. Additionally, it is
obvious that the resistance to liquid/water permeation and
hydrophobicity of SiR and epoxy composites decreases
by increasing the temperature (100ºC).
Moreover, in the early stage of immersion, increase in
temperature leads to higher mass-uptake as confirmed by
SiR composites immersed in varying concentration of
NaCl solutions at 65ºC [36]. The variation in mass uptake
of polymer blends may be due to enough free volume at
higher temperature (i.e. higher water diffusion-
coefficient), which absorb more water molecules to move
inward andthereby increases the net sample weight [22].
Overall, it can be inferred, that micro-SiO2 filled epoxy
blends showed higher immersion/penetration resistance
compared to SiR samples. The goal of this work was to
examine the effect of silica (micro/nano-size) particles on
liquid-permeation/water-immersion resistance of silicone
rubber and epoxy composites. In this regard, the detail
optimization is in progress and will be reported in future.
Fig.6. 02 h boiling-water immersion results of SiR and Epoxy
composites
IV. CONCLUSION
In this paper, the influence of micro/nano-SiO2 on 24h
and 02h boiling water immersion/permeation resistance
of SiR and epoxy composites were investigated using
ASTM-D570 standard procedure.Considerable influence
of SiO2particles incorporation on water immersion
resistance of SiR and epoxy blends was noted.
24h immersion test reveals that compared to SiR and
other investigated specimens, the micro-SiO2 filled epoxy
(EPm) blend showed higher immersion resistance (10mg
mass uptake), whereas the epoxy/nano-SiO2 blend (EPn)
indicated minimum immersion resistance (80mg mass
gain). Likewise, the 02h boiling water immersion test
results revealed that the potency of SiR and Epoxy blends

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to mass uptake was varied with temperature as well as
fillers concentration in polymer matrix. Moreover, among
all investigated blends, the minimum mass uptake of ~01
mg was noticed for neat SiR (SR0), whereas maximum
mass uptake of ~200 mg was found for epoxy/micro-SiO2
sample. These results suggest that the micro-SiO2 filled
epoxy composites possess higher immersion resistance
than SiO2 filled SiR composites.
The findings of this work will provide evidence for
industry that the SiO2 modified polymer dielectrics can
be effectively used to develop HV insulants with higher
liquids immersion/penetration resistance.
ACKNOWLEDGMENT
The authors would like to acknowledge the valuable
suggestions of Prof. Raji Sundararajan of Purdue
University, USA.
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