Peculiarities of near-electrode relaxation processes in the polyethylene melt filled with graphite and carbon black
By using the oscilloscope method within the frequency range 10 to 10⁶ Hz at the temperature 492.1 K and pressure 11.31 MPa at the output of the single-screw extruder, the dielectric properties of the composite melt – linear low-density polyethylene + 20 wt.% of graphite + 10 wt.% of carbon black – h...
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Kuryptya, Ya.A. Savchenko, B.M. Kovalchuk, O.V. Kovalchuk, T.M. Shostak, T.S. 2017-06-14T17:52:29Z 2017-06-14T17:52:29Z 2016 Peculiarities of near-electrode relaxation processes in the polyethylene melt filled with graphite and carbon black / Ya.A. Kuryptya, B.M. Savchenko, O.V. Kovalchuk, T.M. Kovalchuk, T.S. Shostak // Semiconductor Physics Quantum Electronics & Optoelectronics. — 2016. — Т. 19, № 3. — С. 290-294. — Бібліогр.: 20 назв. — англ. 1560-8034 DOI: 10.15407/spqeo19.03.290 PACS 77.22.Ch,Gm, 81.40.Tv https://nasplib.isofts.kiev.ua/handle/123456789/121602 By using the oscilloscope method within the frequency range 10 to 10⁶ Hz at the temperature 492.1 K and pressure 11.31 MPa at the output of the single-screw extruder, the dielectric properties of the composite melt – linear low-density polyethylene + 20 wt.% of graphite + 10 wt.% of carbon black – have been investigated. It has been shown that in the whole frequency range, near-electrode processes significantly effect on charge transfer. For the frequencies less than 100 Hz, in the near-electrode area the conductance is provided with hopping movement of electrons. For the frequencies over 100 Hz, charge transfer occurs through the ion movement. It has been shown that the transfer of ions in the near-electrode area can be described using the relaxation process that, unlike the vast majority of processes described in the publications, meets the wellknown relations only in terms of the complex conductivity. It has been shown that, in the terms of the complex conductivity, this relaxation process can be approximated with Debye equation, as well as it has been estimated the relaxation time (8.5 ms) for this process. According to the parameters included in the Debye equation, it has been estimated the thickness of the near-electrode area (17 μm) and shown that it practically coincides with the sizes of graphite particles. The work shows the results of investigation in accord with the scientic program “Development of an integrated method of forming the ergonomic and functional and operational characteristics of footwear, haberdashery products, special (for servicemen) and domestic purposes” (16/04/52 ДБ) Ministry of Education and Science of Ukraine. en Інститут фізики напівпровідників імені В.Є. Лашкарьова НАН України Semiconductor Physics Quantum Electronics & Optoelectronics Peculiarities of near-electrode relaxation processes in the polyethylene melt filled with graphite and carbon black Article published earlier |
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Peculiarities of near-electrode relaxation processes in the polyethylene melt filled with graphite and carbon black |
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Peculiarities of near-electrode relaxation processes in the polyethylene melt filled with graphite and carbon black Kuryptya, Ya.A. Savchenko, B.M. Kovalchuk, O.V. Kovalchuk, T.M. Shostak, T.S. |
| title_short |
Peculiarities of near-electrode relaxation processes in the polyethylene melt filled with graphite and carbon black |
| title_full |
Peculiarities of near-electrode relaxation processes in the polyethylene melt filled with graphite and carbon black |
| title_fullStr |
Peculiarities of near-electrode relaxation processes in the polyethylene melt filled with graphite and carbon black |
| title_full_unstemmed |
Peculiarities of near-electrode relaxation processes in the polyethylene melt filled with graphite and carbon black |
| title_sort |
peculiarities of near-electrode relaxation processes in the polyethylene melt filled with graphite and carbon black |
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Kuryptya, Ya.A. Savchenko, B.M. Kovalchuk, O.V. Kovalchuk, T.M. Shostak, T.S. |
| author_facet |
Kuryptya, Ya.A. Savchenko, B.M. Kovalchuk, O.V. Kovalchuk, T.M. Shostak, T.S. |
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2016 |
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Semiconductor Physics Quantum Electronics & Optoelectronics |
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Інститут фізики напівпровідників імені В.Є. Лашкарьова НАН України |
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Article |
| description |
By using the oscilloscope method within the frequency range 10 to 10⁶ Hz at the temperature 492.1 K and pressure 11.31 MPa at the output of the single-screw extruder, the dielectric properties of the composite melt – linear low-density polyethylene + 20 wt.% of graphite + 10 wt.% of carbon black – have been investigated. It has been shown that in the whole frequency range, near-electrode processes significantly effect on charge transfer. For the frequencies less than 100 Hz, in the near-electrode area the conductance is provided with hopping movement of electrons. For the frequencies over 100 Hz, charge transfer occurs through the ion movement. It has been shown that the transfer of ions in the near-electrode area can be described using the relaxation process that, unlike the vast majority of processes described in the publications, meets the wellknown relations only in terms of the complex conductivity. It has been shown that, in the terms of the complex conductivity, this relaxation process can be approximated with Debye equation, as well as it has been estimated the relaxation time (8.5 ms) for this process. According to the parameters included in the Debye equation, it has been estimated the thickness of the near-electrode area (17 μm) and shown that it practically coincides with the sizes of graphite particles.
|
| issn |
1560-8034 |
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https://nasplib.isofts.kiev.ua/handle/123456789/121602 |
| citation_txt |
Peculiarities of near-electrode relaxation processes in the polyethylene melt filled with graphite and carbon black / Ya.A. Kuryptya, B.M. Savchenko, O.V. Kovalchuk, T.M. Kovalchuk, T.S. Shostak // Semiconductor Physics Quantum Electronics & Optoelectronics. — 2016. — Т. 19, № 3. — С. 290-294. — Бібліогр.: 20 назв. — англ. |
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2025-11-26T13:13:39Z |
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2025-11-26T13:13:39Z |
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| fulltext |
Semiconductor Physics, Quantum Electronics & Optoelectronics, 2016. V. 19, N 3. P. 290-294.
doi: 10.15407/spqeo19.03.290
© 2016, V. Lashkaryov Institute of Semiconductor Physics, National Academy of Sciences of Ukraine
290
PACS 77.22.Ch,Gm, 81.40.Tv
Peculiarities of near-electrode relaxation processes
in the polyethylene melt filled with graphite and carbon black
Ya.A. Kuryptya1, B.M. Savchenko1, O.V. Kovalchuk1, T.M. Kovalchuk2, T.S. Shostak
1Kyiv National University of Technologies and Design, Kyiv, Ukraine
2V. Lashkaryov Institute of Semiconductor Physics, National Academy of Sciences of Ukraine, Kyiv, Ukraine
E-mail: akoval@knutd.com.ua
Abstract. By using the oscilloscope method within the frequency range 10 to 106 Hz at
the temperature 492.1 K and pressure 11.31 MPa at the output of the single-screw
extruder, the dielectric properties of the composite melt – linear low-density polyethylene
+ 20 wt.% of graphite + 10 wt.% of carbon black – have been investigated. It has been
shown that in the whole frequency range, near-electrode processes significantly effect on
charge transfer. For the frequencies less than 100 Hz, in the near-electrode area the
conductance is provided with hopping movement of electrons. For the frequencies over
100 Hz, charge transfer occurs through the ion movement. It has been shown that the
transfer of ions in the near-electrode area can be described using the relaxation process
that, unlike the vast majority of processes described in the publications, meets the well-
known relations only in terms of the complex conductivity. It has been shown that, in the
terms of the complex conductivity, this relaxation process can be approximated with
Debye equation, as well as it has been estimated the relaxation time (8.5 ms) for this
process. According to the parameters included in the Debye equation, it has been
estimated the thickness of the near-electrode area (17 μm) and shown that it practically
coincides with the sizes of graphite particles.
Keywords: polyethylene, graphite, carbon black, conductance, dielectric properties, near-
electrode relaxation process, single-screw extruder.
Manuscript received 12.04.16; revised version received 14.07.16; accepted for
publication 13.09.16; published online 04.10.16.
1. Introduction
Currently, polymer composites are widely used in
various fields of technology. Therefore, to expand their
functionality, studies are performed using different types
of polymers and fillers [1-8]. In recent years for such
studies, the use of nanoparticles is typical [9-10].
It is clear that the properties of polymer composites
will essentially depend on the polymer material. For
specific tasks, it is not always necessary to look for new
materials, but polymers long been synthesized can be
used. These polymers include polyethylene [11-12]. The
interest to this material will increase significantly, as
most recently it was disclosed broad applicability of
polyethylene in nanoporous form for making clothes,
which by its parameters (thermal conductivity and
moisture permeability) exceeds the natural material such
as cotton [13]. Beside polyethylene as a separate
material, it is important to create composites based on
polyethylene with the desired properties. The necessary
properties can be better provided with polyethylene or
composites based on it, if to expand the conditions of
controlling the material parameters directly in the
technological process.
For the majority of the works analyzed by us from
the viewpoint of properties inherent to composites based
on polyethylene, it is typical that the physical properties
of these materials are investigated after the
polymerization process. This made it impossible to
intervene into the process, especially when the quality of
Semiconductor Physics, Quantum Electronics & Optoelectronics, 2016. V. 19, N 3. P. 290-294.
doi: 10.15407/spqeo19.03.290
© 2016, V. Lashkaryov Institute of Semiconductor Physics, National Academy of Sciences of Ukraine
291
Fig. 1. Scheme for manufacturing and research of dielectric properties of polyethylene melt with impurities of graphite and carbon
black in extruder: 1 – drive of extruder; 2 – extruder, 3 – adapter for measuring the electrical conduction of the polymer melt with
electrodes for measurement; 4 – heads of the extruder with forming filament extrusion device, 5 – device for measuring the
resistance and capacitance by using the oscilloscope method within the wide frequency range.
polyethylene or filler does not meet the required
parameters in accordance with the technological chart of
the process. When manufacturing the composite
materials, it is very important to provide uniformity of
distribution of impurities over the whole polymer bulk.
It can be definitely evaluated when studying the
dielectric properties of material during the technological
process. To make the task of research closer to real
technological conditions in industry, it is important to
use several components of different properties for
manufacturing composites based on polyethylene.
One of the main methods for preparation of
homogeneous polymers or composites based on them is
extrusion. Therefore, the purpose of this work was to
study dielectric properties of melt of polyethylene
composite with graphite filler and carbon black at the
final stage of manufacturing in the extruder.
2. Materials and methods
To produce the composite powder, we used powdered
linear low-density polyethylene. The concentration of
polyethylene in the composite was 70 wt.%. The main
(by weight) impurity was graphite (colloid specimen,
grade C-1, carbon content of 99.3%, made in Ukraine).
The form of graphite particles was like pebbles:
spherical, elongated. The particle size was within 2.3 to
50 μm. The graphite concentration in the composite
was 20 wt.%.
One more impurity used for creating the composite
was carbon black (PUREBLACK SCD-205 (USA)). The
average size of the carbon black particles was equal to
42 nm, and specific surface area is 50 m2/g. The
concentration of graphite in the composite was 10 wt.%.
We produced the composite based on polymer,
graphite and carbon black by using single-screw
extruder with the diameter 25 mm. The main elements of
the extruder are schematically depicted in Fig. 1.
A cell for measuring the resistance R and
capacitance C were mounted into the extruder head. Its
construction is shown in Fig. 2. The distance between
electrodes was d = 1 mm. The area of the electrodes was
equal to S = 5.72 mm2.
The dielectric properties of the obtained sandwich
cells were studied within the frequency range 10 to 106 Hz
at the temperature 293 K by using the oscilloscopic
method [14]. Oscillograms were photographed using a
digital camera, and then their treatment was held. This
made it possible to significantly speed up the measure-
ment process, which was very important for these studies.
The amplitude of the measuring signal with
sinusoidal shape was 0.4 V. Assuming that the
equivalent circuit of the measuring cell is connected in
parallel to the resistance and capacitor, we determined
the value of resistance R and capacitance C of the
samples at different frequencies.
The study was performed using the method
developed by us for measuring electrical properties of
the polymer melt during its processing as described in
the patent [15]. The method is to measure the dielectric
properties of the polymer in the molten state at
processing temperature by using two electrodes in the
form of thin rods that are placed in the extruder after the
dosing zone. The mixture of composite components is
loaded to the extruder hopper after its transition to the
viscous-flow state and homogenization, at the end of the
third zone of the extruder, in the mounted adapter the
dielectric parameters being measured.
Our research has shown that during the first
extrusion and partly during the second one, the meterage
has changed over time. Therefore, the study of
composites within the frequency range was performed
starting from the third extrusion.
In this work, the data were analyzed for seventh
extrusion. Technological process parameters for this
extrusion are given in Table.
Semiconductor Physics, Quantum Electronics & Optoelectronics, 2016. V. 19, N 3. P. 290-294.
doi: 10.15407/spqeo19.03.290
© 2016, V. Lashkaryov Institute of Semiconductor Physics, National Academy of Sciences of Ukraine
292
Fig. 2. The structure of the cell to study the dielectric
properties of polyethylene melt with graphite and carbon black.
1 – adapter, 2 – internal channel of adapter, 3 – mounting holes
of adapter, 4 – spark plugs built into the adapter, 5 – electrical
contacts of spark plugs, 6 – gap between the electrodes in the
inner channel of adapter.
Table. Parameters of the technological process for the
seventh extrusion of polyethylene composite with graphite
and carbon black.
Te
m
pe
ra
tu
re
in
th
e
fil
lin
g
zo
ne
(z
on
e
1)
, K
Te
m
pe
ra
tu
re
in
th
e
pl
as
tic
at
io
n
zo
ne
(z
on
e
2)
, K
Te
m
pe
ra
tu
re
in
th
e
do
si
ng
z
on
e
(z
on
e
3)
, K
Sp
ee
d
of
re
vo
lu
tio
ns
pe
r s
ec
on
d
of
sc
re
w
,
re
v/
s
Te
m
pe
ra
tu
re
in
th
e
zo
ne
o
f
m
ea
su
re
m
en
ts
, K
Pr
es
su
re
in
th
e
zo
ne
of
m
ea
su
re
m
en
ts
,
M
Pa
437 473 483 8.49 492.1 11.31
3. Results and discussion
Our analysis of the measured frequency dependences of
resistance and capacitance has shown that dispersion of
R and C is observed almost in the whole range of
frequencies f. It is known [16-18] that analysis of the
frequency dependences of R and C is performed using
the dielectric spectroscopy methods. In dielectric
spectroscopy, the analysis of these dependences is
mainly made in the terms of complex permittivity ε*:
ε* = ε' – i ε'', (1)
where ε' – real and ε'' – imaginary components of
complex permittivity.
The frequency dependences ε' (1) and ε'' (2) of
polyethylene melt with impurities of graphite and carbon
black are shown in Fig. 3.
As follows from the analysis of the data, the value
ε' is higher than 10 for f < 105 Hz and is equal to 1000 at
the frequencies near f ≈ 103 Hz. As we have shown in
[19, 20], these large ε' quantities are caused by
inhomogeneous distribution of the electric field in the
sample due to the impact of near-electrode processes.
Therefore, these large ε'quantities can be cosidered as
the effective ones. In [19, 20], we have also shown as the
dispersion of ε' and ε'', which is caused by the influence
of near-electrode processes, is described by the same
relations that the dispersion in the bulk of samples
(Debye dispersion, Cole–Cole dispersion, etc.).
The analysis of data in Fig. 3 shows that, in the
terms of the complex permittivity, dispersion of ε' and ε''
is not described by any of the known laws.
As shown in [18], dispersion of R and C on the
frequency of measuring signal can be also analyzed in
the terms of the complex conductance:
σ* = σ' + i σ'', (2)
where σ' – real and σ'' – imaginary components of the
complex conductance. In this case,
σ' = ε0
ω ε'' (3)
and
σ'' = ε0
ω ε', (4)
where ε0 is the electric constant, and ω = 2π f is the
cyclic frequency.
The frequency dependences σ' (1) and σ'' (2) for
polyethylene melt with the impurities of graphite and
carbon black are shown in Fig. 4.
101 102 103 104 105
100
101
102
103
104
105
ε
f, Hz
1
2
Fig. 3. Frequency dependences of the real ε′ (1) and imaginary
ε′′ (2) components of complex permittivity of polyethylene
melt with impurities of graphite and carbon black. The melt
temperature is 219.1 °C, the pressure in the measuring area is
11.31 MPa.
101 102 103 104 105
10-5
10-4
σ,
O
hm
-1
m
-1
f, Hz
1
2
Fig. 4. Frequency dependences of the real σ′ (1) and imaginary
σ′′ (2) components of complex conductance of polyethylene
melt with impurities of graphite and carbon black. The melt
temperature is 492.1 °C, the pressure in the measuring area is
11.31 MPa.
Semiconductor Physics, Quantum Electronics & Optoelectronics, 2016. V. 19, N 3. P. 290-294.
doi: 10.15407/spqeo19.03.290
© 2016, V. Lashkaryov Institute of Semiconductor Physics, National Academy of Sciences of Ukraine
293
0.0000 0.0002 0.0004
0.0000
0.0001
0.0002
0.0003
σ"
, O
hm
-1
m
-1
σ', Ohm-1m-1
Fig. 5. Cole–Cole diagram (dependence σ″(σ′)) for the data
presented in Fig. 4.
Unlike the data presented in Fig. 3, the plots in
Fig. 4 correspond to the known laws for relaxation
processes. To assertain the type of relaxation process in
accord with the data shown in Fig. 4, we constructed and
analyzed the Cole–Cole diagram. In the case of complex
conductance, it corresponds to the dependence σ' (σ'')
that is graphically depicted in Fig. 5.
As follows from Fig. 5, the dependence σ' (σ'') can
be approximated by a semicircle. According to the
theory of relaxation processes [16-18], this dispersion in
the terms of the complex conductance can be considered
as the Debye dispersion and described by the relation
ti
s
ω+
σ−σ
+σ=σ ∞
∞
∗
1
, (5)
σ∞ is the conductance value at f = ∞, σs – conductance
value at f = 0, and τ – relaxation time. Estimations of the
σ∞ and σs values from the Cole–Cole diagrams are as
follows: σ∞ = 1.4·10–5 and σs = 4.1·10–4 Ohm–1m–1. We
estimate the value of the relaxation time: τ = 8.5 ms.
Being based on the permittivity ε∞ value at f = ∞
and εs one at f = 0 in the work [19], from the expression
s
dl
ε
ε
= ∞
2
(6)
we have first estimated (based on dielectric spectroscopy
data) the thickness of near-electrode area l, in which the
relaxation process occurs.
Our analysis indicates that, in the case of
considerating the causes of dispersion of R and C on the
frequency in the terms of complex conductance, for
estimation of the thickness of near-electrode area one
can use the formula similar to the equation (6), namely:
s
dl
σ
σ
= ∞
2
. (7)
The thickness of the near-electrode area evaluated
on the basis of the relation (7) is 17 μm. From the
comparison of the l value with particle sizes of graphite
and carbon black, one can assume that blocking the
exchange of charge on the interface ‘melt of composite –
electrode’ is caused by graphite, the particle size of which
is comparable with the l value. It may be also suggested
that for the frequencies f > 102 Hz the electrical current in
the melt is provided by the transfer of ions. These mobile
ions can be both separate uncontrolled ions that may be
contained in each component of the composite and ions
adsorbed on the surface of carbon black nanoparticles.
Much larger particles of graphite can limit the process of
interaction between these ions and electrodes. As a
result, the electric field is mainly applied to the near-
electrode areas.
As it follows from Fig. 5, at the frequencies f <
102 Hz (right wing in the Cole–Cole diagram) there is a
significant deviation from the circle. It can be explained
by the presence of the electron component of
conductance, except the mechanism of ionic charge
transfer through the melt composite. For the case of a
disordered structure that is the composite under study,
these charge transfer can not be considered on the basis
of the band model developed for the ordered solids, but
can be considered as hopping transfer of electrons in the
model of disordered structures. Certain time is necessary
to make the hop. Therefore, at the frequencies higher
than the reciprocal value of this time, the charge transfer
efficiency by using electrons becomes very low. Taking
into accout that the deviation of the Debye law (equation
(5)) begins at the frequencies 100 Hz, we can assume
that for hopping of electron from one article of carbon
black to another, it takes time no less than 10 ms.
4. Results and conclusions
By using the oscilloscope method within the frequency
range 10 to 106 Hz at the temperature 492.1 K and
pressure 11.31 MPa at the output of the single-screw
extruder, dielectric properties of the composite
consisting of linear low-density polyethylene, 20 wt.%
of graphite and 10 wt.% of carbon black have been
investigated. It has been shown that in the whole
frequency range, dispersion of R and C on the
frequency is observed. From the analysis of the
frequency dependences of components of complex
permittivity, it has been concluded that for the whole
frequency range the electric field is mainly applied to
the near-electrode areas.
It has been shown that the relaxation process, by
using which dispersion of resistance and capacitance
can be described, cannot be approximated being based
on the terms of the complex dielectric permittivity,
because it does not correspond to any of already
described in publications (Debye dispersion, Cole–Cole
dispersion, etc.). The detailed analysis of the relaxation
process determined experimentally has shown that it
can be described by the Debye equation, but in the
terms of the complex conductance. Estimated have
been the value of the relaxation time (8.5 ms) and the
thickness of near-electrode area (17 μm), in which the
relaxation process occurs.
Semiconductor Physics, Quantum Electronics & Optoelectronics, 2016. V. 19, N 3. P. 290-294.
doi: 10.15407/spqeo19.03.290
© 2016, V. Lashkaryov Institute of Semiconductor Physics, National Academy of Sciences of Ukraine
294
Since the thickness of the near-electrode area
matches the sizes of the graphite particles, it was
assumed that blocking the exchange of charge between
charge carriers and electrodes occurs due to the graphite
particles adsorbed on the electrode surface. It has been
also assumed that the Debye equation describes the
transfer of ions of uncontrolled impurities of both
individual particles and those bound with nanoparticles
of carbon black.
It has been shown that deviation from the Debye
law for the frequencies below 100 Hz can be explained
by contribution of the electron component of
conductance into charge transfer in the near-electrode
area. For disordered structure, which is polymer melt,
this charge transfer can occur hoppingly. Since the
electron mechanism of transfer becomes effective for the
frequencies below 100 Hz, it gives the value of time not
less than 10 ms to transfer electrons.
Acknowledgements
The work shows the results of investigation in accord
with the scientic program “Development of an integrated
method of forming the ergonomic and functional and
operational characteristics of footwear, haberdashery
products, special (for servicemen) and domestic
purposes” (16/04/52 ДБ) Ministry of Education and
Science of Ukraine.
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