Structure and Raman spectra of (Cu₆PS₅I)₁₋ₓ(Cu₇PS₆)ₓ mixed crystals
Mixed (Cu₆PS₅I)₁₋ₓ(Cu₇PS₆)ₓ crystals were grown using a direct crystallization technique. Being based on the X-ray diffraction data, their crystal structure was studied, showing a face-centred cubic lattice for Cu₆PS₅I-rich solid solutions (х ‹ 0.12) and a primitive cubic lattice for Cu₇PS₆-rich (0....
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Інститут фізики напівпровідників імені В.Є. Лашкарьова НАН України
2017
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| Cite this: | Structure and Raman spectra of (Cu₆PS₅I)₁₋ₓ(Cu₇PS₆)ₓ mixed crystals / I.P. Studenyak, M.M. Luchynets, V.Yu. Izai, A.I. Pogodin, O.P. Kokhan, Yu.M. Azhniuk, D.R.T. Zahn // Semiconductor Physics Quantum Electronics & Optoelectronics. — 2017. — Т. 20, № 3. — С. 369-374. — Бібліогр.: 15 назв. — англ. |
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Digital Library of Periodicals of National Academy of Sciences of Ukraine| _version_ | 1860272245555855360 |
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| author | Studenyak, I.P. Luchynets, M.M. Izai, V.Yu. Pogodin, A.I. Kokhan, O.P. Azhniuk, Yu.M. Zahn, D.R.T. |
| author_facet | Studenyak, I.P. Luchynets, M.M. Izai, V.Yu. Pogodin, A.I. Kokhan, O.P. Azhniuk, Yu.M. Zahn, D.R.T. |
| citation_txt | Structure and Raman spectra of (Cu₆PS₅I)₁₋ₓ(Cu₇PS₆)ₓ mixed crystals / I.P. Studenyak, M.M. Luchynets, V.Yu. Izai, A.I. Pogodin, O.P. Kokhan, Yu.M. Azhniuk, D.R.T. Zahn // Semiconductor Physics Quantum Electronics & Optoelectronics. — 2017. — Т. 20, № 3. — С. 369-374. — Бібліогр.: 15 назв. — англ. |
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| container_title | Semiconductor Physics Quantum Electronics & Optoelectronics |
| description | Mixed (Cu₆PS₅I)₁₋ₓ(Cu₇PS₆)ₓ crystals were grown using a direct crystallization technique. Being based on the X-ray diffraction data, their crystal structure was studied, showing a face-centred cubic lattice for Cu₆PS₅I-rich solid solutions (х ‹ 0.12) and a primitive cubic lattice for Cu₇PS₆-rich (0.84 ‹ x ‹ 1) solid solutions. These structural data correlate with the Raman spectra, where, besides the common features typical for the argyrodite-type Cu₆PS₅I and Cu₇PS₆ crystals, weaker bands characteristic only for the end-point compounds are revealed in the corresponding compositional intervals.
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| first_indexed | 2026-03-21T11:51:02Z |
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Semiconductor Physics, Quantum Electronics & Optoelectronics, 2017. V. 20, N 3. P. 369-374.
doi: https://doi.org/10.15407/spqeo20.03.369
© 2017, V. Lashkaryov Institute of Semiconductor Physics, National Academy of Sciences of Ukraine
369
PACS 78.40.Ha; 77.80.Bh
Structure and Raman spectra
of (Cu6PS5I)1–x(Cu7PS6)x mixed crystals
I.P. Studenyak1, M.M. Luchynets1, V.Yu. Izai1, A.I. Pogodin1, O.P. Kokhan1, Yu.M. Azhniuk1,2, D.R.T. Zahn3
1Uzhhorod National University, Faculty of Physics,
3, Narodna Sq., 88000 Uzhhorod, Ukraine
2Institute of Electron Physics, NAS of Ukraine, 88000 Uzhhorod, Ukraine
3Semiconductor Physics, Chemnitz University of Technology, D-09107 Chemnitz, Germany
E-mail: studenyak@dr.com
Abstract. Mixed (Cu6PS5I)1–x(Cu7PS6)x crystals were grown using a direct crystallization
technique. Being based on the X-ray diffraction data, their crystal structure was studied,
showing face-centred cubic lattice for Cu6PS5I-rich solid solutions (х < 0.12) and
primitive cubic lattice for Cu7PS6-rich (0.84 < x < 1) solid solutions. These structural data
correlate with the Raman spectra where, besides the common features typical for the
argyrodite-type Cu6PS5I and Cu7PS6 crystals, weaker bands characteristic only for the
end-point compounds are revealed in the corresponding compositional intervals.
Keywords: solid electrolytes, mixed crystals, crystal structure, Raman scattering.
Manuscript received 20.05.17; revised version received 10.07.17; accepted for
publication 06.09.17; published online 09.10.17.
1. Introduction
Cu6РS5I and Cu7PS6 compounds are solid electrolytes of
the argyrodite family [1, 2]. At room temperature, they
crystallize in the cubic crystal system ( mF 34 and P213
space groups, respectively). While Cu6РS5I has been
investigated more extensively [3, 4], the studies of
Cu7PS6 are very scarce [5–7]. At low temperatures, the
Cu6РS5I crystal undergoes two phase transitions (PTs),
one of them being a first-order superionic and
ferroelastic PT at TI = 144–169 K, another is a second-
order structural PT at ТII = (269±2) K [8, 9].
The phase diagram of a quasi-binary Cu2S–P4S10
system was studied in [5]. Cu7PS6 compound is formed
with a large excess of S2– anions, and in a simplified
case its structure can be viewed as a Cu2S matrix
containing isolated [PS4]3– ions. In Cu7PS6, PT is
observed at 515 K from the high-temperature phase with
mF 34 symmetry to the low-temperature phase with P213
symmetry. Calorimetric studies of Cu7PS6 showed no
phase transitions within the temperature range 100 to
400 K, the linear temperature dependence of specific
heat capacity being an evidence for strong
anharmonicity [6].
In this paper, we report on growth technology,
crystal structure and Raman scattering in
(Cu6PS5I)1–x(Cu7PS6)x mixed crystals.
2. Experimental
(Cu6PS5I)1–x(Cu7PS6)x mixed crystals were grown using
the direct crystallization technique from the melt
(Bridgman–Stockbarger method). Synthesis of
(Cu6PS5I)1–x(Cu7PS6)x compounds was performed by the
following procedure: heating at a rate of 50 K/h to
(673 ± 5) K, ageing at this temperature for 24 h, then
heating of the “hot” zone to (1330 ± 5) K and the “cold”
zone to (973 ± 5) K, ageing at this temperature for 72 h
Semiconductor Physics, Quantum Electronics & Optoelectronics, 2017. V. 20, N 3. P. 369-374.
doi: https://doi.org/10.15407/spqeo20.03.369
© 2017, V. Lashkaryov Institute of Semiconductor Physics, National Academy of Sciences of Ukraine
370
and further heating of the melting zone up to
(1380 ± 5) K (50 K above the melting point) with 24 h
ageing. Seeding was performed for 48 h in the lower part
of the container. The crystallization front rate was
3 mm/day. The ampoule with the crystal was
subsequently annealed in the “cold” zone at (973 ± 5) K
for 48 h. As a result, (Cu6PS5I)1–x(Cu7PS6)x single
crystals with the length 45–50 mm and diameter 10–
12 mm were obtained.
Based on the experimental X-ray diffraction data,
measured using a DRON 4-07 diffractometer, the atom
coordinates in the (Cu6PS5I)1–x(Cu7PS6)x mixed crystal
cells were obtained, and the mechanism of the S→I
substitution was clarified. The calculations were
performed using EXPO 2014 software [10, 11].
Micro-Raman studies were performed at room
temperature using a Horiba LabRAM spectrometer with
a CCD camera and a 632.8 nm He-Ne laser. The spectral
resolution was better than 2.5 cm–1.
3. Results and discussion
Typical examples of X-ray diffraction patterns of the
(Cu6PS5I)1–x(Cu7PS6)x solid solutions are shown in
Fig. 1. Based on the X-ray diffraction data, the
crystalline structure of the mixed crystals of Cu6PS5I–
Cu7PS6 system was built based on adjusted models of the
initial structures using the well-known Rietveld
refinement method [12, 13]. Cu6PS5I compound
crystallizes in the face-centred cubic cell ( mF 34 space
group, а = 9.736(1) Å, the number of formula units
Z = 4) [1].The structure is formed by [PS4], [S3I], and
[SI4] tetrahedra, on the faces and in the middle of which
copper atoms are located (Fig. 2a). For Cu6PS5I, the
[PS4] tetrahedron is symmetrical (Fig. 2b) with S2–S2
distance of 3.351 Å and P–S2 distance of 2.052 Å, its
volume being calculated as 4.44 Å3.
Copper atoms in the Cu6PS5I structure are
distributed over nearly equivalent positions of two kinds
Cu1 and Cu2 (24 h and 48 g Wyckoff positions).
Hopping of copper atoms between these positions is the
factor responsible for the ionic conductivity of Cu6PS5I
[1-4]. The conductivity is determined by triangularly
coordinated Cu1 copper atoms located in the center of
CuS3I2 doubled tetrahedra.
In the Cu7PS6 structure (Р213 space group), the
anion core is formed by four kinds of sulphur atoms
(Fig. 3a), the [PS4] tetrahedra are distorted (Fig. 3b). The
phosphorus atom is displaced towards the S2S2S2 plane
and the S–S distances are not equal: the S2–S2 distance
is 3.395 Å, the S2–S3 is 3.251 Å). The P–S distances for
the two kinds of sulphur atoms are 2.029 Å (P–S2),
2.068 Å (P–S3). The [PS4] tetrahedron volume for this
structure is 4.31 Å3.
For mixed (Cu6PS5I)1–x(Cu7PS6)x crystals, it is
essential to consider separately Cu6PS5I-rich and
Cu7PS6-rich compounds, since from our recent study [7]
it follows that (Cu6PS5I)1–x(Cu7PS6)x solid solutions do
not form a continuous compositional row, existing only
in the 0 < х < 0.12 and 0.84 < x < 1 intervals. Due to the
eutectic type of interaction in the Cu6PS5I–Cu7PS6
system (with the х = 0.3 eutectic point coordinate), the
intermediate range (0.12 < х < 0.84) corresponds to the
coexistence of these two phases.
For Cu6PS5I-rich solid solutions (0 < х < 0.12), the
S3 (4a) sulphur atoms are substituted by iodine atoms
without displacement (Fig. 4a). The [PS4] tetrahedron
(Fig. 4b), similarly to Cu6PS5I, remains symmetrical
with the S2–S2 distances of 3.267 Å, the P–S2 distances
of 2.001 Å, and the tetrahedron volume of 4.11 Å3. The
data were calculated for the (Cu6PS5I)0.9(Cu7PS6)0.1
compound.
Fig. 1. X-ray diffraction patterns of the (Cu6PS5I)1–x(Cu7PS6)x
mixed crystals.
Semiconductor Physics, Quantum Electronics & Optoelectronics, 2017. V. 20, N 3. P. 369-374.
doi: https://doi.org/10.15407/spqeo20.03.369
© 2017, V. Lashkaryov Institute of Semiconductor Physics, National Academy of Sciences of Ukraine
371
Fig. 2. Structure of the cubic cell (a) and the [PS4] tetrahedron (b) for Cu6PS5I. Violet circles denote iodine atoms, while blue-and-
white circles denote the nearly equivalent positions of copper atoms, the extent of the blue colour corresponding to the site
occupancy.
Fig. 3. Structure of the cubic cell (a) and the [PS4] tetrahedron (b) for Cu7PS6. Blue-and-white circles denote the nearly equivalent
positions of copper atoms, the extent of the blue colour corresponding to the site occupancy.
Semiconductor Physics, Quantum Electronics & Optoelectronics, 2017. V. 20, N 3. P. 369-374.
doi: https://doi.org/10.15407/spqeo20.03.369
© 2017, V. Lashkaryov Institute of Semiconductor Physics, National Academy of Sciences of Ukraine
372
Fig. 4. Structure of the cubic cell (a) and the [PS4] tetrahedron (b) for (Cu6PS5I)0.9(Cu7PS6)0.1. Violet circles denote iodine atoms
while blue-and-white circles denote the nearly equivalent positions of copper atoms, the extent of the blue colour corresponds to
the site occupancy.
Fig. 5. Structure of the cubic cell (a) and the [PS4] tetrahedron (b) for (Cu6PS5I)0.15(Cu7PS6)0.85. Blue-and-white circles denote the
nearly equivalent positions of copper atoms, the extent of the blue colour corresponds to the site occupancy. White S4 circles are
partly coloured violet denoting partial substitution with iodine.
For the Cu7PS6-rich solid solutions (the composi-
tional range 0.84 < x < 1) with Р213 structure, sulphur is
replaced with iodine in the S4 (4а) positions. For the
nearly limiting case of (Cu6PS5I)0.15(Cu7PS6)0.85, the
[PS4] tetrahedron is distorted due to the asymmetry of
the S–S bonds (the S2–S2 distance is 3.347 Å, the S2–S3
one is 3.194 Å) and a displacement of the phosphorus
atom towards the S2S2S2 plane (Fig. 5). The corres-
pondding P–S distances are 2.029 Å (P–S2) and 1.923 Å
(P–S3), the [PS4] tetrahedron volume is 4.11 Å.
Despite the great number of atoms in the unit cell,
the room-temperature Raman spectrum of Cu6PS5I
Semiconductor Physics, Quantum Electronics & Optoelectronics, 2017. V. 20, N 3. P. 369-374.
doi: https://doi.org/10.15407/spqeo20.03.369
© 2017, V. Lashkaryov Institute of Semiconductor Physics, National Academy of Sciences of Ukraine
373
single crystal (the bottom curve in Fig. 6) is known to
contain a relatively small number of vibrational bands
[14], which can be related to the fact that some of them,
being close in frequency, can be resolved only at lower
temperatures. Besides, the lower-frequency bands
corresponding to the vibrations of more weakly bound
iodine and copper atoms can be masked by the Rayleigh
scattering tail. The dominating feature is a narrow
(7 cm–1) peak at 420 cm–1 corresponding to a symmetric
vibration of the PS4 tetrahedra. A less intense, much
broader (39 cm–1) peak at 308 cm–1 results from the
unresolved degenerated E and F2 bands assigned to
bending vibrations of the PS4 tetrahedral groups [14, 15].
A weaker band observed at 539 cm–1 is ascribed to
internal stretching vibrations of the PS4 tetrahedra [14].
As can be seen from the topmost curve in Fig. 6,
for Cu7PS6 the Raman spectrum resembles that of
Cu6PS5I, with a similar dominating narrow (6 cm–1) peak
at 425 cm–1 and a broader (50 cm–1) maximum at
303 cm–1. Since these two compounds are of basically
similar argyrodite structure with the same PS4 tetrahedral
groups, we, similarly to Cu6PS5I [14], can assign the
maxima at 425 and 303 cm–1 in the Raman spectrum of
Cu7PS6 to the symmetric stretching vibrations of the PS4
tetrahedra and their bending vibrations, respectively.
However, there are distinct features that noticeably
distinguish the Cu7PS6 spectrum from that of Cu6PS5I.
A clear lower-frequency maximum is observed at
142 cm–1 as well as a relatively weak shoulder is
resolved at 227 cm–1 (see the topmost curve in Fig. 6).
There are no data regarding any features at close
frequencies for the Raman spectra of Cu6PS5I, Cu6PS5Br
or Cu6PS5Cl crystals although some weak maxima in the
range 100–200 cm–1 were reported [14]. Their nature
cannot be clearly specified yet, most likely these bands
cannot be related to the internal vibrations of the PS4
tetrahedra. With regard to the weaker high-frequency
band observed at 539 cm–1 for Cu6PS5I, there is no
evidence for a similar maximum in the Raman spectrum
of Cu7PS6. One should note that Cu7PS6 is characterized
by a primitive cubic crystal lattice (Р213 space group),
contrary to the face-centred cubic lattice for Cu6PS5I
( mF 34 ), which can be the reason for absence of the
corresponding vibration in the Cu7PS6 spectrum.
The evolution of Raman spectra of the mixed
(Cu6PS5I)1–x(Cu7PS6)x crystal samples with x can be
traced from Fig. 6. For Cu7PS6-rich samples with
x = 0.85 and x = 0.90 the spectra are very much like to
that of Cu7PS6, with the clearly visible peak near
143 cm–1 and weak shoulder near 225 cm–1, and without
any pronounced features around near 540 cm–1. Such
behaviour is consistent with the existence of a
continuous row of crystalline solid solutions in this
compositional range (0.84 < x < 1) with Р213 structure.
Meanwhile, with further increasing the Cu6PS5I content
(decreasing x) in the Raman spectra of the solid
solutions, one can observe a maximum in the range 530–
540 cm–1, while the features near 143 and 225 cm–1
vanish. It correlates with the data of the structural studies
[7] showing that in the broad intermediate range the
Cu7PS6-like phase of the Р213 structure coexists with the
Cu6PS5I-like phase of the mF 34 symmetry group, and
the features typical for the latter are revealed in the
Raman spectra.
Fig. 6. Room-temperature Raman spectra of (Cu6PS5I)1–
x(Cu7PS6)x crystals measured under the excitation with
λexc = 632.8 nm.
Semiconductor Physics, Quantum Electronics & Optoelectronics, 2017. V. 20, N 3. P. 369-374.
doi: https://doi.org/10.15407/spqeo20.03.369
© 2017, V. Lashkaryov Institute of Semiconductor Physics, National Academy of Sciences of Ukraine
374
4. Conclusions
Mixed (Cu6PS5I)1–x(Cu7PS6)x crystals were grown using
the direct crystallization technique. Based on the X-ray
diffraction data, their crystal structure has been studied,
showing face-centred cubic lattice for Cu6PS5I-rich solid
solutions (х < 0.12) and primitive cubic lattice for
Cu7PS6-rich (0.84 < x < 1) solid solutions. This change
of the lattice structure with the heterovalent S→I
substitution occurs due to a distortion of the [PS4]
tetrahedron.
Despite the basic similarity of the Raman spectra of
the argyrodite-type Cu6PS5I and Cu7PS6 crystals, re-
latively weak bands typical only for Cu6PS5I (539 cm–1)
and Cu7PS6 (143 and 226 cm–1) end-point compounds
have been revealed. The maxima at 143 and 226 cm–1
have been also observed for the mixed (Cu6PS5I)1–
x(Cu7PS6)x crystals of the Cu7PS6-rich compositional
interval (0.84 < x < 1), which, together with the absence
of the high-frequency band at 539 cm–1, clearly
correlates with the Р213 structure of the Cu7PS6-rich
phase. The band at 539 cm–1 observed for the
intermediate (Cu6PS5I)1–x(Cu7PS6)x compositional range
with the coexisting Р213 and mF 34 phases correlates
with the Cu6PS5I-type face-centred structure.
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| id | nasplib_isofts_kiev_ua-123456789-214943 |
| institution | Digital Library of Periodicals of National Academy of Sciences of Ukraine |
| issn | 1560-8034 |
| language | English |
| last_indexed | 2026-03-21T11:51:02Z |
| publishDate | 2017 |
| publisher | Інститут фізики напівпровідників імені В.Є. Лашкарьова НАН України |
| record_format | dspace |
| spelling | Studenyak, I.P. Luchynets, M.M. Izai, V.Yu. Pogodin, A.I. Kokhan, O.P. Azhniuk, Yu.M. Zahn, D.R.T. 2026-03-05T12:00:49Z 2017 Structure and Raman spectra of (Cu₆PS₅I)₁₋ₓ(Cu₇PS₆)ₓ mixed crystals / I.P. Studenyak, M.M. Luchynets, V.Yu. Izai, A.I. Pogodin, O.P. Kokhan, Yu.M. Azhniuk, D.R.T. Zahn // Semiconductor Physics Quantum Electronics & Optoelectronics. — 2017. — Т. 20, № 3. — С. 369-374. — Бібліогр.: 15 назв. — англ. 1560-8034 PACS: 78.40.Ha; 77.80.Bh https://nasplib.isofts.kiev.ua/handle/123456789/214943 https://doi.org/10.15407/spqeo20.03.369 Mixed (Cu₆PS₅I)₁₋ₓ(Cu₇PS₆)ₓ crystals were grown using a direct crystallization technique. Being based on the X-ray diffraction data, their crystal structure was studied, showing a face-centred cubic lattice for Cu₆PS₅I-rich solid solutions (х ‹ 0.12) and a primitive cubic lattice for Cu₇PS₆-rich (0.84 ‹ x ‹ 1) solid solutions. These structural data correlate with the Raman spectra, where, besides the common features typical for the argyrodite-type Cu₆PS₅I and Cu₇PS₆ crystals, weaker bands characteristic only for the end-point compounds are revealed in the corresponding compositional intervals. en Інститут фізики напівпровідників імені В.Є. Лашкарьова НАН України Semiconductor Physics Quantum Electronics & Optoelectronics Structure and Raman spectra of (Cu₆PS₅I)₁₋ₓ(Cu₇PS₆)ₓ mixed crystals Article published earlier |
| spellingShingle | Structure and Raman spectra of (Cu₆PS₅I)₁₋ₓ(Cu₇PS₆)ₓ mixed crystals Studenyak, I.P. Luchynets, M.M. Izai, V.Yu. Pogodin, A.I. Kokhan, O.P. Azhniuk, Yu.M. Zahn, D.R.T. |
| title | Structure and Raman spectra of (Cu₆PS₅I)₁₋ₓ(Cu₇PS₆)ₓ mixed crystals |
| title_full | Structure and Raman spectra of (Cu₆PS₅I)₁₋ₓ(Cu₇PS₆)ₓ mixed crystals |
| title_fullStr | Structure and Raman spectra of (Cu₆PS₅I)₁₋ₓ(Cu₇PS₆)ₓ mixed crystals |
| title_full_unstemmed | Structure and Raman spectra of (Cu₆PS₅I)₁₋ₓ(Cu₇PS₆)ₓ mixed crystals |
| title_short | Structure and Raman spectra of (Cu₆PS₅I)₁₋ₓ(Cu₇PS₆)ₓ mixed crystals |
| title_sort | structure and raman spectra of (cu₆ps₅i)₁₋ₓ(cu₇ps₆)ₓ mixed crystals |
| url | https://nasplib.isofts.kiev.ua/handle/123456789/214943 |
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