Homogeneity ranges of Tl5Te2Cl and Tl 5Te2Br

Article abstract of DOI:10.1134/S0020168508100087

This paper systematizes phase-diagram data for the Tl-TlCl(Br)-Te systems and presents their 500-K subsolidus phase diagrams. Tl₅Te ₂Cl and Tl₅Te₂Br (Tl₅Te₃ structure) are shown to be nonstoichiometric compounds with wide homogeneity ranges, which have been accurately determined using emf measurements, x-ray diffraction, and microhardness tests. Using emf data for reversible concentration cells with a thallium electrode, we have evaluated the partial thermodynamic functions of the thallium in the alloys studied, the standard thermodynamic functions of formation of Tl₅Te₂Cl and Tl₅Te₂Br, and their standard entropies. The crystal chemistry of these phases of variable composition is discussed in relation to the Tl₅Te₃ structure.

Full text of DOI:10.1134/S0020168508100087

ISSN 0020-1685, Inorganic Materials, 2008, Vol. 44, No. 10, pp. 1069–1075. © Pleiades Publishing, Ltd., 2008.
Original Russian Text © M.B. Babanly, M.I. Chiragov, Yu.A. Yusibov, 2008, published in Neorganicheskie Materialy, 2008, Vol. 44, No. 10, pp. 1196–1202.
*
Homogeneity Ranges of Tl5Te2Cl and Tl5Te2Br
M. B. Babanly, M. I. Chiragov, and Yu. A. Yusibov
Baku State University, ul. Khalilova 23, Baku, AZ1148 Azerbaijan
e-mail: babanly_mb@rambler.ru
Received September 14, 2007
Abstract—This paper systematizes phase-diagram data for the Tl–TlCl(Br)–Te systems and presents their
500-K subsolidus phase diagrams. íl5íÂ2ël and íl5íÂ2Çr (íl5íÂ3 structure) are shown to be nonstoichiomet-
ric compounds with wide homogeneity ranges, which have been accurately determined using emf measure-
ments, x-ray diffraction, and microhardness tests. Using emf data for reversible concentration cells with a thal-
lium electrode, we have evaluated the partial thermodynamic functions of the thallium in the alloys studied, the
standard thermodynamic functions of formation of íl5íÂ2ël and íl5íÂ2Çr, and their standard entropies. The
crystal chemistry of these phases of variable composition is discussed in relation to the íl5íÂ3 structure.
DOI: 10.1134/S0020168508100087
*
INTRODUCTION
(íl5íÂ3 structure, sp. gr. I4/mcm) with the following
lattice parameters:
The Tl–X–Hal (X = Se, Te; Hal = Cl, Br, I) systems
have been studied extensively by several groups [1–8].
The pseudobinary joins TlHal–Tl2Se and ílI–í12íÂ
were shown to contain ternary compounds of the
Tl5X2Hal stoichiometry [1–3], which crystallize in the
íl5íÂ3 structure (tetragonal symmetry, sp. gr. I4/mcm)
[4]. The above ternary systems were studied in the com-
position regions Tl–TlHal–Se [5–7] and Tl–TlI–Te [3].
The results were used to construct T–x phase diagrams
along a number of joins, several isothermal sections,
and liquidus diagrams.
‡ = 8.921 Å, Ò = 12.690 Å, z = 4 (Tl5Te2Cl);
‡ = 8.926 Å, Ò = 12.801 Å, z = 4 (í15íÂ2Çr).
The íl5íÂ2ël(Çr) compounds were shown to form
a continuous series of solid solutions with íl5íÂ3 [10].
It is of interest to note that the ílël(Çr)–íl2í and
Tl5Te3–Tl5Se2Cl(Br) systems contain not only wide
solid-solution ranges but also liquid–liquid miscibility
gaps. The T–x phase diagrams of the TlCl(Br)–Te sys-
tems feature monotectic and degenerate eutectic equi-
libria [11]. The other joins studied, TlCl(Br)–
TlTe(íl2íÂ3) and íl5íÂ2ël(Çr)–ílí are not pseudo-
binary: at least one end-member in these systems melts
incongruently [12–15]. The subsolidus phase relations
in these systems are, however, stable: the alloys consist
of mixtures of the end-members. Only in the last two
systems were limited solid solutions identified (based
on íl5íÂ2ël(Çr), with a limit at ꢀ15 mol % TlTe [12,
13].
The ternary compounds Tl5Se2Hal and Tl5Te2I are
known to have wide homogeneity ranges, which extend
well beyond the TlHal–Tl2Se and TlI–Tl2Te pseudobi-
nary systems. In earlier studies [5, 6, 8], emf measure-
ments were used to evaluate the standard thermody-
namic functions of formation of these thallium chalco-
genides.
The lack of data on thallium telluride chlorides and
thallium telluride bromides led our group to undertake
a detailed study of the phase equilibria in the Tl–Te–
Cl(Br) systems along several joins [9–15]. The pseudo-
binary systems TlCl(Br)–Tl2Te were shown to contain
ternary compounds with the compositions Tl5Te2Cl and
Tl5Te2Br, which melt incongruently by syntectic reac-
tions at 708 and 750 K, respectively [9]. Both com-
pounds are phases of variable composition.
This paper describes our attempt to obtain a com-
plete picture of the phase equilibria in the Tl–TlCl(Br)–
Te systems, to more accurately determine the homoge-
neity ranges of the ternary compounds íl5íÂ2ël(Çr),
and to evaluate the thermodynamic functions of their
formation.
EXPERIMENTAL
According to powder x-ray diffraction (XRD) data,
these compounds crystallize in tetragonal symmetry
For our experiments, we synthesized the com-
pounds TlCl, TlBr, íl2íÂ, ílíÂ, íl5íÂ3, íl2íÂ3,
íl5íÂ2ël, and íl5íÂ2Çr. The thallium tellurides were
prepared by melting high-purity (99.99%) thallium and
tellurium at 750 K in silica tubes sealed off under a vac-
*
Presented in part at the XII Conference High-Purity Substances
and Materials: Preparation, Analysis, and Application, Nizhni
Novgorod, Russia, May 28–31, 2007.
1069

1070
BABANLY et al.
uum of ~10–2 Pa. Given that TlTe and íl2íÂ3 form per-
itectically at 573 and 511 K, respectively [16], these
compounds were homogenized at 550 and 500 K for
200 and 300 h, respectively.
functions of composition in the range 66.7–100 mol %
íl2íÂ, confirming that íl5íÂ2ël and íl2í form a con-
tinuous series of solid solutions.
According to XRD data, the solid solutions contain-
ing 66.7–88 mol % Tl2Te (δ−phase) are isostructural
with íl5íÂ2ël, and those containing ≥90 mol % íl2íÂ
(α phase) are similar in XRD pattern to íl2í (mono-
clinic structure, sp. gr. ë2/Ò [20]). The α + δ two-phase
region is essentially degenerate (Fig. 1a, dashed lines).
We assume that, at ꢀ90 mol % íl2íÂ, there is an
TlCl and TlBr were prepared by an indirect process,
as described elsewhere [17]. First, metallic thallium
was dissolved in dilute (5%) H2SO4 at ꢀ350 K to give
a Tl2SO4 solution. To a boiling 2% Tl2SO4 solution was
added dilute HCl or HBr until complete precipitation.
After cooling, the TlCl was separated from the solution,
washed with distilled water, and dried for a long time at
110–120°ë in a drying cabinet. Since TlBr is difficult
to recrystallize, the mother liquor was removed by
repeated boiling with water, followed by suction filtra-
tion. The material was dried in a desiccator over KOH
at 390–400 K and stored in the dark (to avoid its
decomposition).
The ternary compounds íl5íÂ2ël and íl5íÂ2Çr were
synthesized by vacuum-melting a stoichiometric mix-
ture of TlCl(Br) and íl2íÂ. Since these compounds
decompose into two immiscible liquids on melting [9],
the ampule containing the melt was cooled very slowly
(over a period of 5 h) from 800 to 700 and 740 K,
respectively (temperatures intermediate between those
of the syntectic and eutectic equilibria in the
ílël−íl2í and ílÇr–íl2í systems), and held there
for ꢀ 200 h.
α
δ morphotropic transition.
In going from 98 mol % íl2í to íl5íÂ2ël, the
microhardness of the solid solutions decreases, sug-
gesting that the stoichiometric compound íl5íÂ2ël has
the least distorted crystal lattice [18].
In the composition range <66.7 mol % íl2íÂ, the
microhardness of the δ phase and the emf are composi-
tion-independent, in accordance with the constant
phase composition of the system and the constant com-
positions of the coexisting phases.
In the ílÇr–íl2í system, we found other solid-
state phase relations (Fig. 2). The XRD, emf, and
microhardness data for this system indicate the exist-
ence of an α + δ two-phase region (ꢀ80–92 mol %
íl2íÂ).
Detailed characterization of thoroughly annealed
alloys, especially in the composition regions íl2í–
íl5íÂ2ël(Çr)–ílíÂ, enabled us to construct the 500-K
subsolidus phase diagrams of the Tl–TlCl(Br)–Te sys-
tems. It can be seen in Fig. 3 that TlCl, the most ther-
modynamically stable compound in the Tl–TlCl–Te
system, plays a key role in determining the phase rela-
tions in this system. The field of the íl5íÂ2ël-based
phase (δ) is bounded by the íl5íÂ2-ıëlı (0 < ı < 1) com-
positions on the Te-rich side and by the ílël–íl2í join
on the Tl-rich side. The íl2í–íl5íÂ2ël–íl5–íÂ3 com-
position triangle contains an α + δ two-phase region,
which narrows down in going from the Tl–Te constitu-
ent system to the morphotropic phase boundary in the
ílël−íl2í join.
All of the synthesized compounds were identified
by differential thermal analysis (DTA) and XRD.
Tl–TlCl(Br)–Te samples were prepared by melting
the above compounds with Tl and Te in evacuated silica
tubes, followed by prolonged (400–500 h) annealing at
temperatures 30–50 K below the solidus. The samples
were characterized by DTA (NTR-70 pyrometer,
Chromel–Alumel thermocouples), XRD (DRON-2
powder diffractometer, ëuäα radiation), microhard-
ness measurements (PMT-3 tester) [18], and emf mea-
surements using concentration cells of the type
(–)Tl(s)
pglycerol + äHal
(1)
+ TlHal (TlHal–Tl2Te–Te)(s)(+)
In Fig. 3, we indicate the 300-K emf values (mV) for
some of the three-phase regions. The emf is composi-
tion-independent within each of these regions and
changes jumpwise in going from one region to another.
Note that the emf in the ílël–ílí–íl2íÂ3 and ílël–
íl2íÂ3–í three-phase regions coincides to within
3 mV with the values reported by Vasil’ev et al. [21]
for TlTe and íl2íÂ3, respectively. This lends support to
the subsolidus phase diagram under consideration and
indicates that there are no significant ranges of TlTe- or
íl2íÂ3-based solid solutions.
at temperatures from 300 to 430 K. The emf was mea-
sured by a compensation technique with a V-7-34A
high-resistance digital voltmeter. The procedures used
to set up electrochemical cells and measure their emf
were similar to those described earlier [5, 6, 9].
RESULTS AND DISCUSSION
To check the earlier reported phase diagrams of the
ílël(Çr)-íl2í systems [9], we studied these systems
using emf and microhardness measurements. The
results are presented in Figs. 1 and 2, together with the
T–x phase diagrams.
The subsolidus phase diagram of the Tl–TlBr–Te
system is similar to that in Fig. 3, with the only differ-
ence that the α + δ two-phase region in the Br system is
Figure 1 demonstrates that, in the ílël–íl2í system,
the microhardness and the emf of cell (1) are continuous somewhat broader.
INORGANIC MATERIALS Vol. 44 No. 10 2008

HOMOGENEITY RANGES OF Tl5Te2Cl AND Tl5Te2Br
1071
E, mV (300 K)
(c)
417
400
300
230
(b)
1450
H, åP‡
1400
1300
(a)
L
1
T, K
L + L
1
2
L
2
708
703
700
L + δ
2
L + δ
1
692
693
690
680
e
δ
TlCl + Tl Te Cl
5
2
α
20
40
60
80
TlCl
Tl Te
2
mol %
Fig. 1. (a) T–x, (b) H–ı, and (c) E–x diagrams of the ílël−íl í system.
2
Thus, the thallium telluride halides with the íl5íÂ3 Tl16(TlTe2Hal)4 [9]. Their unit cell results from halogen
structure are typical nonstoichiometric compounds. To substitution for the Te(2) atoms residing in the opposite
gain insight into the mechanism underlying the forma- corners of the octahedron along the ë axis (Fig. 4). The
difference in charge between the X2– and Hal– ions is
compensated by the transition of all the thallium atoms
located in the center of the octahedra to the oxidation
state 1+. It is easy to show that such anion substitutions
may, in principle, lead not only to the boundary compo-
sition íl5íÂ2Hal of íl5íÂ3-structured chalcogenides
but also to all íl5íÂ3 – ıHalx (0 < x < 1) intermediate
compositions. The electroneutrality of each composi-
tion is ensured through the transition of an appropriate
fraction of the thallium cations to the oxidation state
1+. This leads to the formation of continuous or wide
series of íl5íÂ3-structured solid solutions in the
Tl−TlHal–Te systems.
tion of the crystal lattice of these compounds and the
formation of íl5íÂ2 – ıHalx solid solutions, consider the
salient features of the íl5íÂ3 structure.
íl5íÂ3 crystallizes in tetragonal symmetry and
forms its own structure type [4], with four formula units
per unit cell. The basic structural component of íl5íÂ3
is a tellurium octahedron with a thallium atom in its
center (Fig. 4). The octahedra share corners to form a
Tl4Te12, or (ílíÂ3)4, framework. The other 16 thallium
atoms per unit cell reside between the octahedra and
link them along the ë axis, forming the Tl16(TlTe3)4
unit cell.
The crystal-chemical formula of the íl5íÂ2Hal
compounds can be represented in the form rately determine the boundaries of phase fields in the
Using emf data, we were able not only to more accu-
INORGANIC MATERIALS Vol. 44 No. 10 2008

1072
BABANLY et al.
E, mV (300 K)
(c)
(b)
434
400
300
230
H, åP‡
1400
1450
1300
(‡)
T, K
L
L
1
L + L
2
1
2
750
750
L + δ
1
733
730
730
L + δ
2
710
690
TlCl + Tl Te ClBr
5
2
697
p
693
δ
α
δ + α
TlBr
20
40
60
80
Tl Te
2
mol %
Fig. 2. (a) T–x, (b) H–x, and (c) E–x diagrams of the TlBr−Tl Te system.
2
TlCl
40
(417)
(439)
(470)
Tl + δ + TlCl
1
20
δ + TlTe
Tl + δ
1
TlCl + Tl Te + Te
2
3
Tl
20
40
δ
TlTe
at % Te
60
Tl Te
2 3
80
Te
α
Tl + α
α + δ
Fig. 3. 500-K section of the Tl–TlCl–Te phase diagram; numbers in parentheses indicate the 300-K emf (mV) for the phase region.
INORGANIC MATERIALS Vol. 44 No. 10 2008

HOMOGENEITY RANGES OF Tl5Te2Cl AND Tl5Te2Br
1073
Tl(1)
Tl(2)
Te(1)
Te(2)
Fig. 4. Basic structural component of Tl Te .
5
3
Tl–TlCl(Br)–Te phase diagrams but also to evaluate the
íl + 0.5ílHal + ílí = 0.5íl5íÂ2Hal.
thermodynamic functions of íl5íÂ2ël and íl5íÂ2Çr.
Therefore, the standard thermodynamic functions of
formation of the ternary compounds can be found using
relations of the form
Table 1 presents linear equations for the tempera-
ture-dependent emf of cell (1) in some of the phase
fields in the Tl–TlCl(Br)–Te systems. The equations
were obtained by least squares fitting our experimental
data [22].
From the data in Table 1, we evaluated partial ther-
modynamic functions of thallium in the alloys using
well-known relations [19] (Table 2).
It can be seen from Fig. 3 that partial molar values
of thallium in the three-phase regions TlHal–
Tl5íÂ2Hal–TlTe are the thermodynamic functions of
potential-forming solid-state reactions of the form
∆G0(Tl5Te2Hal)
= 2∆G(Tl) + ∆G0(TlHal) + 2∆G(TlTe),
where ∆G0 is the standard Gibbs energy, and their stan-
dard entropy can be found as
S0(Tl5Te2Hal) = 2∆S(Tl) + 2S0(Tl)
+ S0(TlHal) + S0(TlTe).
INORGANIC MATERIALS Vol. 44 No. 10 2008

1074
BABANLY et al.
Table 1. Temperature-dependent emf of cell (1) for some of the phase fields in the Tl–TlCl(Br)–Te systems
Phase field in Fig. 3
E (mV) = a + bT 2SE(T)
TlCl–Tl2Te3–Te
461.2 + 0.032T 2[(1.6/22) + 5 × 10–5(T – 361.6)2]1/2
431.8 + 0.035T 2[(0.9/22) + 3 × 10–5(T – 361.6)2]1/2
420.4 – 0.012T 2[(2.4/22) + 7.5 × 10–5(T – 360.4)2]1/2
464.8 + 0.013T 2[(2.2/22) + 6 × 10–5(T – 359.5)2]1/2
434.2 + 0.030T 2[(3.7/22) + 9 × 10–5(T – 359.5)2]1/2
435.5 – 0.003T 2[(1.7/22) + 5.3 × 10–5(T – 360.4)2]1/2
TlCl–TlTe–Tl2Te3
TlCl–TlTe–Tl5Te2Cl
TlBr–Tl2Te3–Te
TlBr–TlTe–Tl2Te3
TlBr–TlTe–Tl5Te2Br
Table 2. Relative partial thermodynamic functions of thalli-
3. Alieva, R.A., Babanly, I.M., Babanly, D.M., and Aliev, I.I.,
T–x–y Phase Diagram of the Tl–TlI–Te System, Khim.
Probl., 2004, no. 4, pp. 83–88.
4. Bhan, S. and Shubert, K., Kristallstruktur von Tl5Te3 and
Tl2Te3, J. Less-Common Met., 1970, vol. 20, no. 3,
pp. 229–235.
5. Babanly, D.M., Yusibov, Yu.A., and Babanly, M.B.,
Phase Diagram and Thermodynamic Properties of the
Tl–TlCl–Se System, Zh. Neorg. Khim., 2007, vol. 52,
no. 5, pp. 819–826.
um in Tl–TlCl(Br)–Te alloys at 298 K
–∆G(Tl) –∆H(Tl)
–∆S(Tl)
Phase field in Fig. 3
kJ/mol
J/(mol K)
TlCl–TlTe–Tl5Te2Cl 40.920
0.122
40.563
0.605
1.198
1.671
TlBr–TlTe–Tl5Te2Br 41.819
0.093
41.733
1.392
0.289
1.41
6. Babanly, D.M., Yusibov, Yu.A., and Babanly, M.B.,
Phase Diagram and Thermodynamic Properties of the
Tl–TlBr–Se System, Zh. Neorg. Khim., 2007, vol. 52,
no. 5, pp. 827–833.
Table 3. Standard thermodynamic functions of thallium tel-
luride halides and input reference data
7. Alieva, R.A., Babanly, I.M., Babanly, D.M., and Aliev,
I.I., Phase Diagram of the Ternary System Tl–Se–I in the
Composition Region Tl–TlI–Se, Vestn. Bakinsk. Univ.,
Ser. Estestv. Nauk, 2004, no. 4, pp. 83–88.
S0(298 K),
–∆G0(298 K) –∆H0(298 K)
Compound
kJ/mol
J/(mol K)
8. Alieva, R.A., Babanly, I.M., Babanly, D.M., and Aliev,
I.I., Thermodynamic Properties of Thallium Selenide
Iodide and Thallium Telluride Iodide, Vestn. Bakinsk.
Univ., Ser. Estestv. Nauk, 2005, no. 1, pp. 42–45.
9. Babanly, D.M., Nadzhafova, A.A., Chiragov, M.I., and
Babanly, M.B., New Thallium Telluride Halides, Khim.
Probl., 2005, no. 2, pp. 149–151.
10. Babanly, D.M., Aliev, I.I.,Yusibov,Yu.A., and Chiragov,
M.I., Tl5Te3–Tl5Te2Cl(Br) Solid Solutions, Azerb. Khim.
Zh., 2007, no. 1, pp. 67–71.
11. Babanly, D.M., Babanly, I.M., Rzaeva, N.A., and
Aliev, I.I., TlCl(Br, I)–Te Pseudobinary Systems, IX
Respublikanskaya nauchnaya konferentsiya po fiziko-
khimicheskomu analizu i neorganicheskomu materia-
lovedeniyu (IX Azeri Conf. on Physicochemical Analy-
sis and Inorganic Materials Research), Baku, 2004, pp.
49–53.
TlCl [23]
TIBr [23]
TITe [21]
Tl5Te2Cl
Tl5Te2Br
Tl5Te2I [8]
185.0 0.8 208.3 3.0 111.5 0.2
167.4 0.6 172.7 0.7 122.6 0.2
44.5 0.4
43.9 0.5 115.9 1.6
355.9 1.1 377.1 5.0 474.1 6.8
340.1 1.0 343.9 4.4 483.4 6.2
296.5 5.3 286.8 3.7
511 8.0
In calculations by these equations, we used refer-
ence data for TlCl, TlBr, TlTe, and Tl (Table 3). Uncer-
tainties were evaluated using error propagation analy-
sis. The results are presented in Table 3.
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