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ABSTRACT
A study on the dielectric spectroscopy of epoxy-based nanocomposites filled with
different types of particles, such as Al2O3, AlN, MgO, SiO2 and BN, is presented. The
surface of the nanoparticles was modified with a silane coupling agent, in order to make
them compatible with the organic host and create a system with homogeneously
dispersed filler material. Morphological characterizations of individual particles and
fabricated composites were performed by means of transmission and scanning electron
microscopy. The present research addresses an analysis of the complex permittivity.
The relative permittivity of nanocomposites shows an unusual behaviour. Introduction
of a low percentage of high permittivity filler results in a decrease of the permittivity of
the bulk polymer material. We propose a qualitative explanation for the reduction of
the relative permittivity, compared to the reference samples. The interface layer of
surface modified particles plays a more important role than the nature of the particles
themselves. The immobilization caused by the surface treatment of the nanoparticles
seems to be the main factor determining the relative permittivity of the composites with
fillgrade below 5 wt.%. The imaginary part of the complex permittivity, which
represents the dielectric losses in the system, does not change significantly with addition
of nanofiller up to 5 wt.%.
Index Terms - Nanocomposite, surface treatment, dielectric spectroscopy, interface
phenomena, relative permittivity.
о OX о OH
о о
Si OX+3H2O Si OH+3XOH
OX OH
Figure 1. Chemical structure of a bisphenol-A type epoxy resin.
Figure 4. Hydrolysis of the GPS.
о
As it is evident from the hydrolysis reaction, the availability
о of free OH-groups on the nanoparticle surface is necessary for
successful surface modification. The particles we use have a
ultrasonication, in order to remove air voids that were trapped The size distribution appeared to be broad for AlN and
during the mixing process. The final composite was cast into Al2O3. However, the fraction of particles with diameters larger
preheated Al-molds and cured at 140 ºC for 4 hours. than 200 nm was negligible. MgO and SiO2 particles had a
ER-SiO2 compounds were not created using this ex-situ narrow size distribution.
polymerization process. The silica nanoparticles were The micrographs of Al2O3 and SiO2 show the shape of the
synthesized inside the epoxy resin. The binary composite particles being spherical. MgO particles have spherical, egg
system of 31.8 wt.% of silica and the ER was diluted to and truncated cubic shapes. AlN particles have spherical,
prepare appropriate concentrations of SiO2. The rest of the hexagonal and cubic structures.
procedure was the same as for the other nanocomposite SEM allows getting an impression of the shape and size
samples, i.e. mixing with hardener, degassing and curing. distribution of microparticles. The shape of BN particles with
The samples prepared for the study have a dimension of 42 70 nm, 1.5 μm and 5 μm is spherical. BN particles with 0.5
mm diameter with 0.5 mm thickness. μm have a platelet-like structure (see Figure 7).
4000 70 nm
0.5 m
3500
1.5 m
5 m
3000
Intensity (a.u.)
2500
2000 Figure 7. TEM micrograph of MgO nanoparticles (left) and SEM micrograph
of BN submicron particles with APS 500 nm (right).
1500
'
-20ºC
properties (i.e. conductivity, permittivity, impedance and 6
-20ºC
Figure 9. A schematic of the DS setup. The sample lies within a cryogenic 0.1
cell, which can be heated up to 400 ºC and cooled down to -160 ºC with 0.01
ºC temperature stability.
3.6
3.4
3.2
'
3.0 Neat ER
MgO-0.5
MgO-2
2.8 MgO-5
Figure 12. A particle without surface modification (left) and a particle with MgO-10
surface modification (right). Grey area around surface treated particle is a
layer of aligned polymer chains.
-2 -1 0 1 2 3 4 5 6 7
10 10 10 10 10 10 10 10 10 10
Frequency (Hz)
Neat ER
3.8 SiO2-0.5
3.2 SiO2-2
SiO2-5
3.6
-2 -1 0 1 2 3 4 5 6 7
10 10 10 10 10 10 10 10 10 10
Frequency (Hz)
3.4
Figure 16. of ER-SiO2 samples as a function of frequency at 20 °C.
'
Neat ER
3.2 Al2O3-0.5
Al2O3-2
The higher values of for Nanopox-based composites,
Al2O3-5 compared to those of neat polymer and composites filled with other
3.0
Al2O3-10 particles are assumed due to the different specimen preparation
-2 -1 0 1 2 3 4 5 6 7
process. Nanopox composites were produced using an in-situ
10 10 10 10 10 10 10 10 10 10
polymerization process. The surface modification is not part of this
Frequency (Hz)
synthesis method, therefore we assume that there is no interfacial
Figure 13. of ER-Al2O3 samples as a function of frequency at 20 °C. layer of aligned polymer chains in the proximity of the SiO2
nanoparticles. Thus, immobilization of epoxy chains does not take
place, which would explain why a reduction of could not be
4.0
observed. Another reason why Nanopox-based composites have
higher relative permittivity values can be due to byproducts, which
3.8 are present inside the polymer after the in-situ precipitation of
nanosilica [24]. These byproducts are assumed to be very mobile
3.6 and lead to a higher of the composite material overall.
The spectra of composite materials containing surface
'
respectively). All (f) curves of ER-MgO have lower values Temperature (ºC)
than those of neat epoxy samples. Since the of the bulk Figure 18. TGA spectra of untreated and GPS treated MgO nanoparticles.
material of MgO, Al2O3 and AlN is approximately the same,
namely 8.5-10 depending on the structure [28-30], we can The relative permittivity values of ER-AlN-5 are higher
conclude that interaction between MgO nanoparticles and host than that of neat ER, while values of ER-Al2O3-5 are still
is the strongest. Since MgO nanoparticles are the smallest, lower. The amount of hydroxyl groups on the surface of
they have the highest surface-to-volume ratio, which leads to alumina is larger than those on the surface of AlN. More GPS
larger amounts of OH groups on the surface. The evidence of groups connect to the surface of Al2O3 particles and in turn
larger amounts of hydroxyl groups on the surface of MgO more dipole groups of epoxy will be immobilized in the
nanoparticles, compared to e.g. Al2O3 nanoparticles, can be interface polymer layer.
found in TGA spectra of as-received and GPS-treated The second effect, which is responsible for the increase of
particles of these types (see Figures 17 and 18). The higher , originates from the relative permittivity of the filler itself.
weight loss for MgO in Figure 18 indicates a higher amount of As the volume of filler material increases, the influence of the
GPS groups that reacted with the OH groups on the surface of material properties of the particles on the of the matrix
the nanoparticles. The reaction of hydroxyl groups with GPS becomes more pronounced. The relative permittivity of all
creates stronger bonds between particles and host. Therefore nanoparticles is higher than the one of ER. The properties of
more dipolar groups will be immobilized in the vicinity of the the filler become predominant at 10 wt.% of Al2O3 or AlN and
MgO nanoparticles. The importance of the size of the particles
therefore (f) has higher values than neat ER. The surface of
and therefore the interface region is underlined by results for
BN-ER composites shown in section 3.4. silica nanoparticles was not modified. That explains why the
AlN particles have the largest APS and therefore smallest relative permittivity of ER-SiO2 systems has higher values at
interface volume. The size of the filler plays an important role. all filler concentrations. The higher volume fraction of the
Since the volume of interfaces decreases for increasing filler filler with higher results in a higher relative permittivity of
size at constant weight percentage, the move to larger filler the system itself.
results in smaller zones of immobilization. The larger the The values of all specimens at 1 kHz and the difference
particles are, the larger the influence of the filler properties compared to neat ER are shown in Table 1. Specimens with
become compared to the changes of the polymer structure and MgO nanoparticles have values between 3.06 and 3.25, which
the influence of the immobilization layers diminishes. is a reduction by 8.5% to 15%, compared to the neat ER. The
IEEE Transactions on Dielectrics and Electrical Insulation Vol. 19, No. 1; February 2012 113
addition of alumina nanofiller leads to a 7.4% reduction as nanoparticles can be used for electrical insulation applications
lowest value of compared to unfilled ER, which has an and the losses are much lower than those of microcomposite
equal to 3.52. The lowest value for ER-AlN composites is 3.4, systems filled with 60 wt.% of conventional sized alumina or
which is a 3.6% reduction. ER-SiO2 samples have a higher silica filler.
compared to reference sample. 3.8
Table 1. The relative permittivity of the specimens at 1 kHz and the difference + 2.5%
compared to neat ER. 3.6
'
- 7.4%
Neat ER - - 3.52 - 3.2
- 15%
ER-Al2O3-0.5 30 (8.5 – 10.0)* 3.41 -3.3 SiO2
ER-Al2O3-2 30 (8.5 – 10.0)* 3.28 -7.4 Neat ER
3.0 AlN-2
ER-Al2O3-5 30 (8.5 – 10.0)* 3.45 -2.0 Al2O3-2
ER-Al2O3-10 30 (8.5 – 10.0)* 3.69 +4.7 MgO-2
2.8
ER-AlN-0.5 60 (8.7 – 8.9)* 3.44 -2.2 10
-2
10
-1
10
0 1
10 10
2 3
10 10
4
10
5
10
6
10
7
* Values for bulk material, depending on the literature source [28-37]. They
might be different for particles of nanometric size.
-2 -1 0 1 2 3 4 5 6
10 10 10 10 10 10 10 10 10
Frequency(Hz)
Figure 19 shows the effect of nanoparticles with a fillgrade
Figure 20. of ER-Al2O3 samples as a function of frequency at 20 °C.
of 2 wt.% on the of the nanocomposites as a function of
frequency. Nanocomposites with 2 wt.% are shown, because
the reduction of is the most pronounced at this fillgrade for
0.1
Neat ER
A2O3 and MgO was treated with GPS, which creates better
adhesion and aforementioned interfacial layer.
The dielectric losses of the composites containing a little
amount of nanoparticles (up to 5 wt.%) do not differ much 0.01
higher than 1 kHz. The polarization of epoxy dipolar groups is Frequency (Hz)
more pronounced in the high frequency region, which causes
Figure 21. of ER-SiO2 samples as a function of frequency at 20 °C.
higher losses in this region. The lower losses of
nanocomposites can be indication for the presence of the
interfacial layer. The side chains, which are responsible for 3.4 EFFECT OF FILLER SIZE
the β-relaxation peak, are restricted in the vicinity of The relative permittivity of epoxy-based compounds with
nanoparticles, while all side chains of unfilled polymer can 10 wt.% of modified micro- and submicron-BN particles is
move in respect to applied field and bring losses to the higher than of the neat ER, while of ER filled with 70 nm
dielectric system. However, at 50 Hz is almost the same particles is lower compared to the reference sample (see
as for ER. That means that ER filled with small amount of Figure 22). XRD analysis showed that the structure of BN is
114 R. Kochetov et al.: Anomalous Behaviour of the Dielectric Spectroscopy Response of Nanocomposites
the same (see Figure 5). Thus, the difference between them illustrated in Figure 24. Smaller particles with the same
could be the size of particles, their aspect ratio and surface weight percentage lead to a larger interfacial volume. In our
modification. The increases if the size of particles case we have a directly proportional relationship between the
increases, while the concentration of them remains constant. overall volume of the interfacial layer and the amount of
polarization. The movement of the dipoles in the layer close to
the particle is restricted. Since the movement of dipoles is
limited, the of the system is lower for smaller particles.
4.4
4.2
4.0
Particle
3.8
'
Interface
3.6
Neat ER Host
3.4
BN-10 5 m
BN-10 1.5 m
3.2
BN-10 0.5 m
BN-10 70 nm Particle/Interface Zone:
3.0
-2 -1 0 1 2 3 4 5 6 7
10 10 10 10 10 10 10 10 10 10
Frequency (Hz)
Figure 24. Illustration of the change of the ratio between particle and interface
volume as a function of particle size [38].
Figure 22. The effect of the filler size on the of composites with 10 wt.%
BN particles for 20 °C as a function of frequency.
The dielectric losses of the samples with 1.5 m and 5 m
The imaginary part of the complex permittivity , which particles have higher values compared to the reference sample.
represents the dielectric losses, is shown in Figure 23. The The of the specimens filled with 70 nm and 0.5 m
dielectric losses of composites filled with BN are higher particles do not differ much compared to neat epoxy.
compared to ER in the low frequency region (<1 kHz) and
lower for frequencies higher than 1 kHz, with exception of 4 DISCUSSION
BN with 5 m APS. The broad dielectric loss peak in the high
frequency region (10 kHz) is attributed to a β relaxation It is generally accepted that the surface-to-volume ratio of
process of the epoxy network. It moves to a higher frequency the nanoscale fillers and the interface-polymer layer in the
with increasing temperature. vicinity of the filler plays a significant role for the decreased
that has been observed [39, 40].
Tanaka et al. [41] proposed the multi-core model, where he
0.1 divided an interfacial layer into 3 layers (bonded, bond and
Neat ER
loose layers). Andritsch [22] proposed the polymer chain
ER-BN-10 (5 m)
ER-BN-10 (1.5 m) alignment model and introduced 2 layers (aligned and
ER-BN-10 (0.5 m) affected). Rätzke & Kindersberger [42] and Todd & Shi [43]
ER-BN-10 (70 nm)
proposed a single interface polymer layer or interphase. All
''
plays a role for the properties of a composite, which is more APS of 70 nm. For the same fillgrade but particles with an
important than the nature of the particles themselves. The total APS 1.5 m, the interface volume will be 0.5%, while for the
interface volume would occupy a larger space if the size of the BN-10 with 5 m particles, this value is reduced to 0.1%. If
particles becomes smaller for the same fillgrade. The treated we make the same calculations, assuming the interface layer
nanoparticles can change the degree of cross-linking, since of 20 nm, then the overall interface volume will occupy 70%,
polymer groups react with SCA molecules, which are grafted 2% and 0.6% for ER-BN-10 (70 nm), ER-BN-10 (1.5 m)
on the surfaces of the nanoparticles. and ER-BN-10 5 (m), respectively (see Figure 25).
The rules of mixture, which are used to predict the relative
permittivity values of composites filled with conventional 10
2
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- nanocomposites”, Proc. Nordic Insul. Sym., Gothenburg, Sweden, pp. Since 1999, he is an Associate Professor in High Voltage Engineering at Delft
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[50] A.S. Vaughan, “On the dielectric response of nanofilled University of Leiden for his research in electro-magnetism
materials”, unpublished. on behalf of the National Science Foundation. He was
employed in different research/management functions
Roman Kochetov was born in 1984 in Kazakhstan during two decades at KEMA’s testing, consultancy and
(USSR). He received the B.Sc. and M.Sc. degrees in engineering company, Arnhem NL. Until 2003 he has been
technique and technology (microelectronics and supervisory board member of the power grid company of
semiconductors) from Saint-Petersburg Electrotechnical South Holland. Since 1996 he is a head of the High Voltage
University with distinction in 2005 and 2007, Technology and Management group at the Delft University
respectively. He participated in exchange two-diploma of technology. In 2004 he has become Director of Education in Electrical Engineering
program and received M.Sc. degree in electrical of the faculty of Electrical Engineering, Mathematics and Computer Science. In 2003
engineering (technical physics) from Lappeenranta he has been the general chairman of the XIII Conference ISH, “International
University of Technology in 2007. His current Ph.D. Symposium on High Voltage Engineering” in Delft and he is currently chairing the
degree research project nanoPOWER has ISH steering committee. He is chairman of the executive board of the KSANDR,
the aim of designing and assessment of new, environmental friendly dielectric organization for Knowledge Sharing and Research in the field of energy
materials, using nanotechnology, to realize insulation components with infrastructures. He represents the Netherlands in the Technical Committee of IEC 98
improved thermal conductivity and electrical breakdown strength. His main on Electrical Insulation Systems. He performs and has performed several functions in
research interests are focused on the nanostructured systems, thermal CIGRÉ, in particular the chairmanship of Study Committee D1, Materials and
conductivity of polymer composites and dielectric spectroscopy of electrical Emerging Technologies. In September 2004 he became honorary member of CIGRÉ,
insulation materials. Paris.