Electrical and dielectrical properties of composites based on (Ag₁₋ₓCuₓ)₇GeS₅I mixed crystals
Polymer composites were prepared from (Ag₁₋ₓCuₓ)₇GeS₅I mixed crystals grown using the Bridgman–Stockbarger method. The impedance measurements were performed at room temperature in the frequency range 10⁻³–2·10⁶ Hz. The frequency dependences of electrical conductivity and dielectric permittivity for...
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Інститут фізики напівпровідників імені В.Є. Лашкарьова НАН України
2018
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| Cite this: | Electrical and dielectrical properties of composites based on (Ag₁₋ₓCuₓ)₇GeS₅I mixed crystals / V.Yu. Izai, V.I. Studenyak, A.I. Pogodin, I.P. Studenyak, M. Rajnak, J. Kurimsky, M. Timko, P. Kopcansky // Semiconductor Physics Quantum Electronics & Optoelectronics. — 2018. — Т. 21, № 4. — С. 387-391. — Бібліогр.: 10 назв. — англ. |
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Digital Library of Periodicals of National Academy of Sciences of Ukraine| _version_ | 1860479655805452288 |
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| author | Izai, V.Yu. Studenyak, V.I. Pogodin, A.I. Studenyak, I.P. Rajnak, M. Kurimsky, J. Timko, M. Kopcansky, P. |
| author_facet | Izai, V.Yu. Studenyak, V.I. Pogodin, A.I. Studenyak, I.P. Rajnak, M. Kurimsky, J. Timko, M. Kopcansky, P. |
| citation_txt | Electrical and dielectrical properties of composites based on (Ag₁₋ₓCuₓ)₇GeS₅I mixed crystals / V.Yu. Izai, V.I. Studenyak, A.I. Pogodin, I.P. Studenyak, M. Rajnak, J. Kurimsky, M. Timko, P. Kopcansky // Semiconductor Physics Quantum Electronics & Optoelectronics. — 2018. — Т. 21, № 4. — С. 387-391. — Бібліогр.: 10 назв. — англ. |
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| container_title | Semiconductor Physics Quantum Electronics & Optoelectronics |
| description | Polymer composites were prepared from (Ag₁₋ₓCuₓ)₇GeS₅I mixed crystals grown using the Bridgman–Stockbarger method. The impedance measurements were performed at room temperature in the frequency range 10⁻³–2·10⁶ Hz. The frequency dependences of electrical conductivity and dielectric permittivity for composites based on (Ag₁₋ₓCuₓ)₇GeS₅I mixed crystals were obtained. The Nyquist plots for (Ag₁₋ₓCuₓ)₇GeS₅I-based composite have been analyzed. The influence of cation Ag→Cu substitution on the electrical conductivity of composites based on (Ag₁₋ₓCuₓ)₇GeS₅I mixed crystals has been studied.
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ISSN 1560-8034, 1605-6582 (On-line), SPQEO, 2018. V. 21, N 4. P. 387-391.
© 2018, V. Lashkaryov Institute of Semiconductor Physics, National Academy of Sciences of Ukraine
387
Hetero- and low-dimensional structures
Electrical and dielectrical properties of composites
based on (Ag1–xCux)7GeS5I mixed crystals
V.Yu. Izai1, V.I. Studenyak1, *, A.I. Pogodin1, I.P. Studenyak1, M. Rajňák2,3, J. Kurimsky3, M. Timko2,
P. Kopčanský2
1
Uzhhorod National University, Faculty of Physics, 3, Narodna Sq., 88000 Uzhhorod, Ukraine
*
E-mail: studenyak@dr.com
2
Institute of Experimental Physics, Slovak Academy of Sciences, Watsonova 47, 040 01 Košice, Slovakia
3
Faculty of Electrical Engineering and Informatics, Technical University of Košice, Letná 9, 04200 Košice, Slovakia
Abstract. Polymer composites were prepared from (Ag1–xCux)7GeS5I mixed crystals grown
using Bridgman–Stockbarger method. The impedance measurements were performed at
room temperature in the frequency range 10–3–2·106 Hz. The frequency dependences of
electrical conductivity and dielectric permittivity for composites based on (Ag1–xCux)7GeS5I
mixed crystals were obtained. The Nyquist plots for (Ag1–xCux)7GeS5I-based composite has
been analyzed. The influence of cation Ag→Cu substitution on electrical conductivity of
composites based on (Ag1–xCux)7GeS5I mixed crystals has been studied.
Keywords: mixed crystals, composites, cation substitution, impedance measurements,
electrical conductivity, dielectric permittivity.
doi: https://doi.org/10.15407/spqeo21.04.387
PACS 78.40.Ha, 77.80.Bh
Manuscript received 29.10.18; revised version received 19.11.18; accepted for publication
29.11.18; published online 03.12.18.
1. Introduction
Ag7GeS5I and Cu7GeS5I crystals belong to the
argyrodite-type superionic conductors and demonstrate
high values of electrical conductivity [1-3]. At room
temperature, they crystallize in the face-centered cubic
lattice ( mF 34 space group, Z = 4); no phase transitions
within the temperature range 77…373 K were observed
[1-3]. Investigations of the influence of cationic
substitution on the physical properties of solid solutions
based on Cu7GeS5I and Ag7GeS5I crystals are only
started. Mechanical properties of (Cu1–xAgx)7GeS5I
mixed crystals studied by micro-indentation method were
presented in Ref. [4]. Crystal growth technology,
electrical and optical properties of other Cu7GeS5I-based
solid solutions were studied in Refs. [5-10].
It should be noted that the crystalline material itself
is very brittle and, thus, not enough applicable in
practice. Solid electrolytes are widely used in the form of
polymer composites in secondary power sources.
Polymer composite form enhances the mechanical
properties of such materials (flexibility, adhesion to
electrodes, etc.). It is expected that at high pressures that
overcome the yield strength of polymer the last one is
pushed out from space between grains and fills the
hollow space. As a result, a better contact between
grains, higher density and better internal adhesion are
achieved.
The paper is aimed at the development of
preparation technology, production of the composites and
study of the electrical and dielectrical properties of
composites based on (Ag1–xCux)7GeS5I mixed crystals.
2. Experimental
Cu7GeS5I-Ag7GeS5I superionic mixed crystals were
obtained by the solid state reaction between finely
grinded and mixed crystalline powders of pure Cu7GeS5I
and Ag7GeS5I taken in corresponding proportions. The
mixtures were sintered at temperature 1173 K during
120 h. As a result, an intensive recrystallization of
material was observed. XRD studies confirmed
formation of continuous series of solid solutions. The
changes of lattice parameter follow the Vegard law.
Polymer composites based on Cu7GeS5I-Ag7GeS5I
mixed crystals were prepared from polycrystalline
powders previously finely grinded in agate mortar. The
obtained powders were ultrasonically dispersed in ethyl
acetate. The solution of EVA bonding polymer (ethylene-
vinyl-acetate copolymer) in ethyl acetate was added to
powder dispersion in amount of 1:9 by mass and further
dispersed in ultrasonic bath for 10 min. Thus, the
composite consisted of 10% of EVA binder and 90% of
superionic active material. The obtained mixture was
SPQEO, 2018. V. 21, N 4. P. 387-391.
Izai V.Yu., Studenyak V.I., Pogodin A.I., et al. Electrical and dielectrical properties of composites based on …
388
evaporated in air with continuous mixing to prevent
sedimentation and enhance the homogeneity of particles.
Then it was dried at 60 °C for 24 h. The dry cake was
grinded in agate mortar and pressed to 8-mm diameter
and hardened with steel mold at room temperature. The
calculated pressure inside the mold was around 7800 bar.
As a result, hard tablets of 8 mm in diameter were
obtained. The electrodes were spray deposited onto both
disk faces by using Cramolin Graphite conductive paint
based on colloidal graphite. Thus, the obtained electrodes
were expected to demonstrate ion blocking effect at DC.
The impedance measurements were performed
within the wide frequency range 10–3…2·106 Hz with no
DC bias and 10 mV AC voltage, applied to the samples.
Agilent E4980A Precision LCR Meter was used for
20…2·106 Hz frequency range. The measurements in
10-3…20 Hz were performed on the lab-scale system.
The analysis of obtained frequency dependences was
made using Scribner ZView software.
3. Results and discussion
The single dispersion region is observed on the frequency
dependences of the real part of electrical conductivity σ′
for composites based on (Ag1–xCux)7GeS5I mixed crystals
(Fig. 1). The low-frequency part is associated with ion
current blocking effect at the “graphite electrode /
superionic composite” interface, while the high-
frequency part of the spectra is defined predominantly by
the charge transfer across the grain boundaries, as will be
shown later. The high-frequency part that is mostly
affected by the internal ionic conductivity of grains isn’t
observed in the frequency range under investigation.
Nevertheless, it demonstrates significant contribution
into frequency behavior in megahertz region and has to
be taken into consideration during fitting. With the
copper content increase, significant attenuation of
dispersion in the low-frequency region can be observed
(Fig. 1), which is caused by the rapid increase of
electronic conductivity as will be shown further.
Fig. 1. Frequency dependences of the real part of electrical
conductivity for composites based on (Ag1–xCux)7GeS5I
mixed crystals: Ag7GeS5I (1), (Ag0.75Cu0.25)7GeS5I (2),
(Ag0.5Cu0.5)7GeS5I (3), (Ag0.25Cu0.75)7GeS5I (4) and Cu7GeS5I
(5).
Fig. 2. Frequency dependences of the real part of electrical
conductivity (1a), imaginary part of impedance (2a), real (1b)
and imaginary (2b) parts of dielectric permittivity for
Ag7GeS5I-based composite.
The sharp increase of imaginary part of impedance
Z′′ in the low-frequency region together with the decrease
of real part of electrical conductivity σ′ (Fig. 2a) is the
evidence of high ionic to electronic conductivity ratio in
composites based on Ag7GeS5I superionic crystals. This
behavior is typical for good solid electrolytes. Two
dispersions can be observed on the frequency
dependences of the real and imaginary parts of dielectric
permittivity for Ag7GeS5I-based composite (Fig. 2b). The
low-frequency dispersion can be associated with
capacitance of the near-electrode layer, while the high-
frequency one can be caused by the capacitance of grain
boundaries.
One large semicircle can be observed in the Nyquist
plot for Ag7GeS5I-based composite (Fig. 3). Its low-
frequency part is defined by the shunt resistance caused
by the electronic conductivity of the sample and
capacitance of the double electric layer capacitor formed
at the interface between the solid electrolyte and graphite
electrode that is irreversible in respect to silver ions. The
high-frequency part of the semicircle is deformed due to
its overlapping with small middle-frequency semicircle
caused by the resistance and capacity of the grain
boundaries. The high-frequency semicircle related to the
internal grain resistivity and bulk capacity of the grains
isn’t observed in the experimental data due to frequency
limitations of the impedance analyzer. Thus, it is shown
only for demonstration purposes as a calculated line
SPQEO, 2018. V. 21, N 4. P. 387-391.
Izai V.Yu., Studenyak V.I., Pogodin A.I., et al. Electrical and dielectrical properties of composites based on …
389
Fig. 4. Nyquist plots for (Ag0.75Cu0.25)7GeS5I (a), (Ag0.5Cu0.5)7GeS5I (b), (Ag0.25Cu0.75)7GeS5I (c) and Cu7GeS5I (d) based composites
with fitting results.
generated by the equivalent circuit used for fitting and
shown in Fig. 3. It is responsible for the high-impedance
shift of the Nyquist plot along Z′ axis. From the
viewpoint of practical interest, the value of the total ionic
conductivity limited by the grain boundary transfer
process can be more interesting in comparison to pure
internal grain conductivity. Thus, the value of resistance
consisting from internal grain and grain boundary
resistances connected in series was used for further
evaluation of the total ionic conductivity of the whole
sample.
Fig. 3. Nyquist plot for Ag7GeS5I-based composite with the
fitting result. A high-frequency magnified part of the plot is
shown in the inset.
In Fig. 4 an evolution of impedance frequency
behavior with increase of copper content in composites
based on (Ag1–xCux)7GeS5I mixed crystals is shown.
Even a small increase in copper content leads to
significant change in proportions of semicircles caused
by sharp increase of parasitic electronic component of
conductivity and moderate decrease of ionic contribution.
The further increase of copper content leads to
degeneration of low-frequency semicircle into the low-
frequency tail that is rather complicate for fitting. The
same equivalent circuit was used for modeling of the
impedance spectra of composite samples with various
copper content. The results of such fitting are
summarized in the table.
Substitution of Ag atoms with Cu ones leads to
sharp increase of electronic component of conductivity
(Fig. 5). The most significant increase is observed at low
copper concentrations that can be considered from the
technological viewpoint as a poisoning effect caused by
Cu impurities in Ag-conducting argyrodite-based solid
electrolytes. Thus, a great attention must be paid to the
traces amount of copper in the silver used in synthesis of
superionic material with high ionic to electronic
conductivity ratio. The decrease of ionic component of
conductivity together with the copper content
increase can be observed in composites based on
(Ag1-xCux)7GeS5I mixed crystals (Fig. 5). The minimum
on the compositional dependence of ionic conductivity
SPQEO, 2018. V. 21, N 4. P. 387-391.
Izai V.Yu., Studenyak V.I., Pogodin A.I., et al. Electrical and dielectrical properties of composites based on …
390
Table. Results of Nyquist plots fitting for composites based on (Ag1–xCux)7GeS5I mixed crystals (Rg and Rgb are grain and grain
boundary resistances; Ri and Re are ionic and electronic resistances; σi and σe are ionic and electronic conductivity; Cg, Cgb and Cdl
are capacitance of the grains, grain boundaries and double electric layer, respectively).
(Ag1–xCux)7GeS5I Rg, Ohm
Rgb,
Ohm
Ri, Ohm
σi,
S/m
Re,
Ohm
σe,
S/m
Cgb, nF Cdl, µF
Cg,
pF
x = 0 407 116 523 1.6·10–1 2.4·108 3.6·10–7 285 0.29 13
x = 0.25 793 1029 1822 2.7·10–2 9707 5.1·10–3 4280 0.69 16
x = 0.5 5357 17794 23151 2.8·10–3 3933 1.7·10–2 3.1 1.54 29
x = 0.75 1272 1438 2710 2.9·10–2 1535 5.1·10–2 16.3 42 46
x = 1 2092 2053 4145 2.0·10–2 262.5 3.2·10–1 251 8.3 24
Fig. 5. Compositional dependences of ionic (1) and electronic
(2) contributions to electrical conductivity for polymer
composites based on (Ag1–xCux)7GeS5I mixed crystals.
The inset shows the compositional dependence of ionic to
electronic conductivity ratio for polymer composites based on
(Ag1–xCux)7GeS5I mixed crystals.
can be explained by the effect of compositional
disordering usually observed in solid solutions [9, 10].
The break of ion conductivity channels caused by the
compositional disordering in crystal lattice leads to the
decrease of ion transport efficiency. It should be noted
that the ratio of ionic to electronic conductivity also
decreases significantly with the increase of copper
content in composites under investigation (inset in
Fig. 5).
4. Conclusions
Cu7GeS5I–Ag7GeS5I superionic mixed crystals were
obtained using the solid state reaction. Polymer
composites based on Cu7GeS5I-Ag7GeS5I mixed crystals
were prepared from the polycrystalline powders and
ethylene-vinyl-acetate binder in proportion 9:1. The
impedance measurements were carried out within the
frequency range 10–3…2·106 Hz.
In the frequency range under investigation, the
single dispersion region in the frequency dependences
of electrical conductivity for composites based on
(Ag1-xCux)7GeS5I mixed crystals has been observed. It
has been shown that the copper content increase leads to
significant attenuation of dispersion in the low-frequency
region, which is caused by the rapid increase of
electronic conductivity. Two dispersions can be observed
in the frequency dependences of dielectric permittivity,
the low-frequency dispersion can be associated with the
capacitance of the near-electrode layer, while the high-
frequency one can be caused by the capacitance of grain
boundaries.
The analysis of obtained frequency dependences
was performed in Scribner ZView software, the Nyquist
plots for composites based on (Ag1–xCux)7GeS5I mixed
crystals were constructed as well as the compositional
dependences of ionic and electronic contributions to
electrical conductivity were discussed. It has been shown
that substitution of Ag atoms with Cu ones leads to a
sharp increase of electronic conductivity, decrease of
ionic conductivity as well as decrease of the ratio of ionic
to electronic conductivity.
Acknowledgments
This work was supported by the Slovak Academy of
Sciences in the framework of projects VEGA
No. 2/0141/16 and project EuroNanoMed-III MAGBRIS.
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Authors and CV
Vitaliy Yu. Izai, born in 1988,
defended his PhD thesis in Physics
and Mathematics in 2013. Senior
Researcher at Uzhhorod National
University. Authored over 35 articles
and 20 patents. The area of scientific
interests is electrical and optical
properties of semiconductors and
superionic conductors.
Uzhhorod National University, Faculty of Physics
Viktor I. Studenyak, born in 1997.
In present time he studies at the
magistracy of Uzhhorod National
University on Faculty of Physics.
Authored 7 articles and 5 patents. The
area of his scientific interests includes
optical properties of superionic conductors.
Uzhhorod National University, Faculty of Physics
Artem I. Pogodin, born in 1988,
defended his PhD thesis in Inorganic
Chemistry in 2016. Senior researcher
of Uzhhorod National University.
Authored over 35 articles and 25
patents. The area of his scientific
interests includes chemistry, solid
state chemistry, crystal growth, materials science.
Uzhhorod National University, Faculty of Physics
Ihor P. Studenyak, Doctor of
Science in Physics and Mathematics,
Professor. Vice-rector for Research at
Uzhhorod National University,
Ukraine. Authored over 200 articles,
115 patents, 15 textbooks. The area
of his scientific interests includes
physical properties of semiconduc-
tors, ferroics and superionic conductors.
Uzhhorod National University, Faculty of Physics
E-mail: studenyak@dr.com
Michal Rajňák, born in 1987,
defended his PhD thesis in Physics of
Condensed Matter in 2015. Currently
he is working as a senior researcher at
Institute of Experimental Physics SAS
focused on dielectric properties of
nanocomposite systems.
Institute of Experimental Physics, Slovak Academy of
Sciences, Košice, Slovakia
Faculty of Electrical Engineering and Informatics,
Technical University of Košice, Košice, Slovakia
Juraj Kurimsky, Doctor of science
in Electrical Power Engineering at
Technical University of Kosice,
assistant professor. Authored over 200
publications. The area of his scientific
interests includes the research of new
dielectric materials, the dielectric
spectroscopy and special
measurements in high voltage technique.
Faculty of Electrical Engineering and Informatics,
Technical University of Košice, Košice, Slovakia
Milan Timko, PhD in solid state
physics. Senior researcher of Institute
of Experimental Physics SAS.
Authored over 220 articles, 4 patents
and 3 textbooks. The area of his
scientific interests includes solid state
physics, magnetic fluids and their
magnetic, dielectric and hyperthermia
properties.
Institute of Experimental Physics, Slovak Academy of
Sciences, Košice, Slovakia
Peter Kopčanský, professor in solid
state physics. Director of Institute of
Experimental Physics SAS. Authored
over 250 articles, 6 patents and 5
textbooks. The area of his scientific
interests includes solid state physics
especially magnetism, transport
properties in disordered systems, magnetic fluids, their
magnetic and dielectric properties and composite systems
with liquid crystals.
Institute of Experimental Physics, Slovak Academy of
Sciences, Košice, Slovakia
|
| id | nasplib_isofts_kiev_ua-123456789-215322 |
| institution | Digital Library of Periodicals of National Academy of Sciences of Ukraine |
| issn | 1560-8034 |
| language | English |
| last_indexed | 2026-03-23T18:47:43Z |
| publishDate | 2018 |
| publisher | Інститут фізики напівпровідників імені В.Є. Лашкарьова НАН України |
| record_format | dspace |
| spelling | Izai, V.Yu. Studenyak, V.I. Pogodin, A.I. Studenyak, I.P. Rajnak, M. Kurimsky, J. Timko, M. Kopcansky, P. 2026-03-12T08:54:46Z 2018 Electrical and dielectrical properties of composites based on (Ag₁₋ₓCuₓ)₇GeS₅I mixed crystals / V.Yu. Izai, V.I. Studenyak, A.I. Pogodin, I.P. Studenyak, M. Rajnak, J. Kurimsky, M. Timko, P. Kopcansky // Semiconductor Physics Quantum Electronics & Optoelectronics. — 2018. — Т. 21, № 4. — С. 387-391. — Бібліогр.: 10 назв. — англ. 1560-8034 PACS: 78.40.Ha, 77.80.Bh https://nasplib.isofts.kiev.ua/handle/123456789/215322 https://doi.org/10.15407/spqeo21.04.387 Polymer composites were prepared from (Ag₁₋ₓCuₓ)₇GeS₅I mixed crystals grown using the Bridgman–Stockbarger method. The impedance measurements were performed at room temperature in the frequency range 10⁻³–2·10⁶ Hz. The frequency dependences of electrical conductivity and dielectric permittivity for composites based on (Ag₁₋ₓCuₓ)₇GeS₅I mixed crystals were obtained. The Nyquist plots for (Ag₁₋ₓCuₓ)₇GeS₅I-based composite have been analyzed. The influence of cation Ag→Cu substitution on the electrical conductivity of composites based on (Ag₁₋ₓCuₓ)₇GeS₅I mixed crystals has been studied. This work was supported by the Slovak Academy of Sciences in the framework of projects VEGA No. 2/0141/16 and project EuroNanoMed-III MAGBRIS. en Інститут фізики напівпровідників імені В.Є. Лашкарьова НАН України Semiconductor Physics Quantum Electronics & Optoelectronics Hetero- and low-dimensional structures Electrical and dielectrical properties of composites based on (Ag₁₋ₓCuₓ)₇GeS₅I mixed crystals Article published earlier |
| spellingShingle | Electrical and dielectrical properties of composites based on (Ag₁₋ₓCuₓ)₇GeS₅I mixed crystals Izai, V.Yu. Studenyak, V.I. Pogodin, A.I. Studenyak, I.P. Rajnak, M. Kurimsky, J. Timko, M. Kopcansky, P. Hetero- and low-dimensional structures |
| title | Electrical and dielectrical properties of composites based on (Ag₁₋ₓCuₓ)₇GeS₅I mixed crystals |
| title_full | Electrical and dielectrical properties of composites based on (Ag₁₋ₓCuₓ)₇GeS₅I mixed crystals |
| title_fullStr | Electrical and dielectrical properties of composites based on (Ag₁₋ₓCuₓ)₇GeS₅I mixed crystals |
| title_full_unstemmed | Electrical and dielectrical properties of composites based on (Ag₁₋ₓCuₓ)₇GeS₅I mixed crystals |
| title_short | Electrical and dielectrical properties of composites based on (Ag₁₋ₓCuₓ)₇GeS₅I mixed crystals |
| title_sort | electrical and dielectrical properties of composites based on (ag₁₋ₓcuₓ)₇ges₅i mixed crystals |
| topic | Hetero- and low-dimensional structures |
| topic_facet | Hetero- and low-dimensional structures |
| url | https://nasplib.isofts.kiev.ua/handle/123456789/215322 |
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