J. Phase Equilib. Diffus.
(2019) 40:697–705
https://doi.org/10.1007/s11669-019-00756-6
Experimental Study of the Binary Nb-Te System
B. S. de Lima1 • N. Chaia1 • L. E. Correa1 • F. S. Oliveira1 • L. R. de Faria1
I. de Oliveira2 • G. C. Coelho1 • A. J. S. Machado1
Submitted: 18 April 2019 / in revised form: 16 September 2019 / Published online: 25 September 2019
Ó ASM International 2019
Abstract Transition metal dichalcogenides have been
receiving considerable attention in the literature due to
their great variety of physical properties. Recently, some
compounds of this family have been pointed out as new
examples of Dirac and Weyl semimetals. However, the
lack of thermodynamic data or experimental studies on
these binary systems makes the synthesis of high-quality
samples purely empirical. This report investigates the
binary Nb-Te phase diagram. Results of x-ray diffraction,
Rietveld refinement, scanning electron microscopy, and
differential thermal analysis strongly suggest that Nb5Te4
and Nb3Te4 are stable only at high temperatures. These
phases decompose according to the following eutectoid
reactions: Nb3Te4(s) ? Nbss ? NbTe2(s) at 735 °C and
Nb5Te4(s) ? Nbss ? Nb3Te4(s) at 839 °C. Furthermore, the
results presented in this study show that NbTe2 and NbTe4
are the only stable compounds in the Te-rich portion of the
phase diagram ([ 60 at.% of Te) at temperatures below
735 °C.
Keywords DTA  Experimental phase equilibria  Nb-Te
system  Nb-tellurides  X-ray diffraction
& B. S. de Lima
delima.bs@gmail.com
1
Escola de Engenharia de Lorena–USP,
P. O. Box 116, Lorena 12602-810, Brazil
2
Combustion and Propulsion Laboratory, National Institute for
Space Research, Cachoeira Paulista, SP 12630-000, Brazil
•
1 Introduction
Over the past decade, transition metal dichalcogenides
(TMDCs) have been the object of many scientific investi-
gations due to their unusual physical properties often
related to the low dimensionality of the crystal structure.
These compounds crystallize in layered structures that are
three atoms thick. These layers are bonded together
through Van der Waals forces between the chalcogen ele-
ments and have been found to host electronic instabilities
such as charge-density waves (CDW) and superconduc-
tivity (SC). Many studies have pointed out that these states
are competitive, as it is the case of 1T-TaS2, 2Ha-MoS2,
and 1T-TiSe2.[1-3] Some compounds even exhibit coexis-
tence of CDW and SC, such as NbSe3, HfTe3, or ZrTe3.[4-9]
More recently, TMDCs have been pointed out as analogs of
graphene due to the presence of Dirac/Weyl fermions in
their electronic structures. Experimental evidence was
found in WTe2, MoTe2, PdTe2 and PtSe2.[10-16] The Nb-Te
system includes some compounds that have been
pointed out as hosts of some of electronics instabilities as
well.[17-26]
Within the phase diagram literature, these transition
metal-chalcogenides have been little studied. According to
ASM Phase Diagram Database,[27] from all the systems
cited here, several are still incomplete regarding their
binary phase diagrams as in the case of Ta-S, Nb-Se, Nb-
Te, Hf-Se, and W-Te. This paper reports new experimental
data of the binary Nb-Te system. Based on x-ray diffraction
(XRD) data, Rietveld analysis, scanning electron micro-
scopy (SEM), and energy dispersive spectroscopy (EDS),
we show that NbTe2 and NbTe4 are the only stable com-
pounds in the Te-rich side of the phase diagram at tem-
peratures below 735 °C. Furthermore, differential thermal
123
698
analysis (DTA) results suggest that Nb5Te4 and Nb3Te4 are
stable at higher temperatures.
2 Literature Review
The literature dedicated to the Nb-Te binary system is very
scarce. To our best knowledge, the study of Smith and
collaborators is the only article that deals with experi-
mental data on this system.[17] They investigated the Te-
rich side of the phase diagram using a Knudsen cell
between 362 and 700 °C. Their results suggest the exis-
tence of three phases between NbTe2 and NbTe4, namely
NbTe3, Nb3Te8, and Nb3Te7. Interestingly, their XRD data
suggests that these phases have crystal structures similar to
the tetragonal NbTe4 (P4/mcc) as it was not possible to
observe significant differences in their XRD patterns.
Furthermore, their results also suggest that NbTe4 (SG P4/
mcc) exists within a solubility range between 76 and
80 at.% of Te. The Nb-Te phase diagram from the ASM
phase diagram database (Fig. 1) is a collection of phases
experimentally determined by x-ray diffraction techniques
or in studies dedicated to their physical properties. The
crystal structure of Nb5Te4 (I4/m) and Nb3Te4 (P63/m)
were first determined by Selte and Kjekshus.[18,19] It was
found that Nb-deficient crystals of Nb5Te4 (SG I4/m)
superconduct below 1 K and exhibit strong magneto-re-
sistance related to strong electron–phonon interactions.[20]
Nb3Te4 is a quasi-one-dimensional conductor with a
Fig. 1 Reproduction of the Nb-
Te binary phase diagram based
on the ASM database.[27]
Spheres represent the
composition and heat-treatment
temperature of 26 samples
discussed in this report
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J. Phase Equilib. Diffus. (2019) 40:697–705
hexagonal symmetry that exhibits coexistence of CDW and
SC.[21]
The crystal structure of NbTe2 was determined by
Brown.[26] This compound crystallizes in a distorted vari-
ant of the 1T-CdI2 prototype structure, with monoclinic
symmetry (C2/m). A similar CdI2-like structure has been
observed for RhTe2 at room temperature.[28] Regarding the
physical properties of NbTe2, Nagata et al. observed a
superconductor ground state below 0.5 K.[22] Recently, this
compound has been studied employing first principle cal-
culations and had its heat of formation calculated as
- 1.38 eV/unit formula.[29] Also, it was shown that its high
electrical conductivity is related to the high carrier density
and high electron mobility, which leads to the low influ-
ence of lattice scattering on electronic transport in this
compound.[29] NbTe4 (SG P4/mcc) is a quasi-one-dimen-
sional conductor due to Nb-Nb chains that form in its
tetragonal symmetry. This compound had its crystal
structure also determined by Selte and Kjekshus.[23] At
room temperature, this compound is in an incommensurate
state that undergoes two successive CDW transitions.[24,25]
Table 1 summarizes the crystallographic data available for
the phases mentioned in this section.
3 Experimental Procedure
Polycrystalline samples were prepared from stoichiometric
mixtures of Nb and Te high purity powders. The mixtures
were homogenized and pressed into pellets that were sealed
J. Phase Equilib. Diffus. (2019) 40:697–705
Table 1 Summary of
Phase label Prototype HMS
crystallographic data of phases
present in the Nb-Te binary NbSS bcc-W Im-3m
system
Nb5Te4 Ti5Te4 I4/m
Nb3Te4 Nb3Te4 P63/m
NbTe2 NbTe2 C2/m
NbTe4 NbTe4 P4/mcc
TeSS k-Se P3121
in quartz tubes under high purity argon and placed in fur-
naces which were heated up at a rate of 100 °C per hour.
Each heat treatment was interrupted by quenching the tubes
in iced water after 48 or 72 h in order to realize an inter-
mediate process of homogenization of the powder. At this
point, the samples were ground into powder, again pressed
into pellets, sealed in quartz tubes, and placed again in the
furnace. The annealing temperature and duration were
defined empirically depending on the region of the phase
diagram that was under analysis; details are given in the
next section. After completing the heat treatment, the
samples were quenched again in iced water. All samples
were analyzed by x-ray diffraction (XRD) in a PANalitycal
Empyrean diffractometer with a PIXcel3D detector using
Cu-Ka radiation. Rietveld refinement was carried out for
all the x-ray diffraction data using the GSAS-II soft-
ware.[30] The refinements were considered reliable when
the error parameter weighted-profile R-factor (Rw) reached
values lower than 10%. SEM images and EDS measure-
ments were obtained in a Hitachi S-3400N SEM (EDAX
AMETEK). Differential thermal analysis (DTA) measure-
ments were carried out in a Netzsch STA 449 F3 under
argon atmosphere with a flow rate of 70 cm3/min, in alu-
mina crucibles with a heating rate of 5 °C/min. Hence, the
estimated uncertainty related to the transition temperature
is 5 °C. During our experiments, no interaction with the
alumina crucibles was observed.
4 Results and Discussion
In this section, we report and discuss the experimental
results of 26 samples. Table 2 summarizes sample com-
positions, heat treatment details, the fraction of each phase
quantified by the Rietveld refinement, and error
parameters.
4.1 Nb-Rich Side
The first set of samples (# 1 to # 6) was annealed at 900 °C
for 96 h in two steps of 48 h. These samples were
homogenized after the first 48 h. Nominal compositions of
these alloys were 0, 0.5, 1.0, 2.5, 5.0 and 10.0 at.% of Te.
699
Cell parameters, Å, ° Refs.
a = b = c = 3.30 a = b = c = 90 33
a = b = 10.23; c = 3.72 a = b = c = 90 18
a = b = 10.67; c = 3.65 a = b = c = 90 19
a = 14.74; b = 3.64; c = 9.37 a = c = 90; b = 110.41 26
a = b = 6.50; c = 6.84 a = b = c = 90 23
a = b = 4.45; c = 5.92 a = b = 90; c = 120 34
The diffractograms obtained after the heat treatment are
presented in Fig. 2. Diffraction peaks related to the Nb5Te4
phase emerges in the sample with a nominal composition
of 1.0 at.% Te and are quantified in the sample with a
nominal composition of 2.5 at.% Te. The intensity of these
peaks increases monotonically, which demonstrates that
the amount of Nb5Te4 increases as expected. The molar
fraction estimated by Rietveld refinement shows that the
amount of Nb5Te4 increases from 0 to 0.45, as one can see
in Table 2. The results presented in Fig. 2 show that at this
temperature all samples are located in a two-phase region
of Nb (Im-3m) and Nb5Te4 (I4/m). These results are in
agreement with the currently accepted Nb-Te phase dia-
gram (Fig. 1).
4.2 Te-Rich Side
Samples # 7 to # 26 were prepared at the Te-rich side of the
phase diagram. The position of each sample in the phase
diagram is shown schematically in Fig. 1. Samples # 7 to #
12 were used to investigate the minimum annealing time
necessary to indicate the probable thermodynamic equi-
librium state. All of these samples have a nominal com-
position 66.67 at.% Te (NbTe2). The XRD data of this set
of samples is shown in Fig. 3. Sample # 7 was heat-treated
at 400 °C for 144 h. Rietveld refinement results show that
the only phase present in this sample is the tetragonal
NbTe4 (P4/mcc). Interestingly, the formation of tetragonal
NbTe4 before monoclinic NbTe2 (C2/m) is closely related
to the Te motion and vacancies in the structure.
The crystal structure of NbTe2 (C2/m) and NbTe4 (P4/
mcc) are closely related if one pictures the crystal structure
as an array in which Nb atoms are surrounded by Te atoms
forming different tridimensional structures. The main dif-
ference is that NbTe4 (P4/mcc) has higher symmetry. As
the data shown in Fig. 3 suggests, a sample prepared with a
nominal composition of NbTe2 and heat-treated at 400 °C
forms first NbTe4 (P4/mcc). Also, the high concentration of
defects in the Te sites has a significant impact on the
electrical properties of this quasi-one-dimensional con-
ductor.[31] The results presented in Fig. 3 shows that the
amount of NbTe2 (C2/m) increases over time, and it is
expected to reach 100%. However, due to the low
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700 J. Phase Equilib. Diffus. (2019) 40:697–705

Table 2 Summary of the Rietveld refinement results

Sample number Composition, at.% Te Temp., °C Duration, h Molar fraction Rw, %
NbSS Nb5Te4 Nb3Te4 NbTe2 NbTe4

1 0 900 96 1 0 0 0 0 8.83
2 0.5 900 96 1 0 0 0 0 8.68
3 1.0 900 96 1 Traces 0 0 0 9.71
4 2.5 900 96 0.88 0.12 0 0 0 9.35
5 5.0 900 96 0.68 0.32 0 0 0 9.06
6 10.0 900 96 0.55 0.45 0 0 0 9.93
7 66.7 400 144 0 0 0 0 1 7.69
8 66.7 400 240 0 0 0 0.09 0.91 9.90
9 66.7 400 408 0 0 0 0.21 0.79 8.69
10 66.7 400 576 0 0 0 0.52 0.48 8.95
11 66.7 400 744 0 0 0 0.58 0.42 8.7
12 66.7 400 912 0 0 0 0.55 0.45 8.78
13 44.4 400 744 0.41 0 0 0.59 0 9
14 57.1 400 744 0.35 0 0 0.65 0 8.99
15 66.7 400 744 0 0 0 0.5 0.5 8.43
16 70 400 744 0 0 0 0.19 0.81 9.18
17 72.7 400 744 0 0 0 0.11 0.89 8.97
18 75 400 744 0 0 0 0.05 0.95 9.2
19 80 400 744 0 0 0 0 1 9.87
20 44.4 500 744 0.44 0 0 0.56 0 7.92
21 57.1 500 744 0.32 0 0 0.68 0 7.99
22 66.7 500 744 0 0 0 0.5 0.5 8.51
23 70 500 744 0 0 0 0.34 0.66 8.71
24 72.7 500 744 0 0 0 0.22 0.78 8.19
25 75 500 744 0 0 0 0.05 0.95 9.71
26 80 500 744 0 0 0 Traces 1 9.28

Fig. 2 XRD data of samples # 1 to # 6. These samples have nominal Fig. 3 XRD data of samples # 7 to # 12 with nominal composition of
composition between 0 and 10 at.% Te and were heat-treated at NbTe2 and different duration of heat treatment at 400 °C
900 °C for 96 h

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temperature involved in these heat treatments, even after
912 h of heat treatment, one can observe a significant
amount of NbTe4 (P4/mcc). Further details of this phe-
nomena are given elsewhere.[31]
After 240 h of heat treatment (sample # 8), monoclinic
NbTe2 (C2/m) starts to form, and diffraction peaks related
to this phase are observed. These peaks are marked by stars
in Fig. 3. By increasing the annealing time, the intensity of
NbTe2 diffraction peaks also increases, suggesting that
tetragonal NbTe4 (P4/mcc) is transforming to monoclinic
NbTe2 (C2/m). The Rietveld refinement shows that the
molar fraction of NbTe4 decreases from 1 to 0.55 after
912 h of heat treatment (Table 2). It is possible to observe
that after 576 h of heat treatment, the phase fractions
obtained by the Rietveld refinement did not change sig-
nificantly. For practical reasons, we have adopted 744 h of
heat treatment for samples # 13 to # 26. Samples # 13 to #
19 were prepared with nominal compositions between 44.4
at.% Te (Nb5Te4) and 80 at.% Te (NbTe4) as pointed out in
Fig. 1. The XRD data for these samples are presented in
Fig. 4.
Phases identified by the Rietveld refinement in samples
# 13 and # 14 (44.4 and 57.1 at.% Te, respectively) were
only NbSS and monoclinic NbTe2 (C2/m). The position of
NbSS peaks is indicated by # in Fig. 4. It is important to
mention that the NbSS peaks were identified by the Rietveld
analysis since their relative intensities are very low. These
results were confirmed by SEM backscattered micrographs,
which are shown in Fig. 5(a) and (b). The darker regions
correspond to NbSS and the brighter regions to NbTe2 for
sample 13. The fraction of NbTe2 increased from 0.59 to
0.65 in samples # 13 to # 14, respectively. Energy Dis-
persive Spectroscopy analysis shows that NbSS has 9 ±1
at.% Te while NbTe2 has 64.8 ±0.5 at.% Te. These results
Fig. 4 XRD data of samples # 13 to # 19 with nominal composition
varying from 44.4 to 80 at.% Te heat-treated at 400 °C for 744 h
701
suggest that the phases Nb5Te4 and Nb3Te4 should only be
stable at higher temperatures since no trace of these phases
were found in the microstructures of samples # 13 and # 14.
Samples # 15 to # 18 exhibit only monoclinic NbTe2 (C2/
m) and tetragonal NbTe4 (P4/mcc) by the Rietveld refine-
ment. In Fig. 5(c), it is possible to observe in the SEM
backscattered micrographs of sample # 16 that the only
phases present in this sample are monoclinic NbTe2 (C2/m)
and NbTe4 (P4/mcc), which is in agreement with the XRD
data. The micrograph of sample # 19, shown in Fig. 5(d),
only exhibits NbTe4 (P4/mcc). The results presented so far
demonstrates that the region from 66.7 to 80 at.% Te is a
two-phase region NbTe2 (C2/m) and NbTe4 (P4/mcc). Our
results did not detect any trace of the intermediate phases
proposed previously.
In order to further characterize this region of the phase
diagram another set of samples, # 20 to # 26, was prepared
with compositions identical to those samples just dis-
cussed; however, the heat treatment was carried out at
500 °C during 744 h. XRD data of these samples are pre-
sented in Fig. 6. The results obtained in the Rietveld
analysis for these samples are very similar to the results of
samples # 13 to # 19. As one can observe in Table 2,
samples # 20 and # 21 have NbSS and monoclinic NbTe2
(C2/m) in their microstructures. By comparing the phase
proportions in composition-equivalent samples treated in
400 and 500 °C, it is possible to notice a significant dif-
ference only between samples with 70 and 72.7 at.% Te.
Samples treated at 500 °C have larger amounts of NbTe2.
This can be explained if the peritectic reaction NbTe3(-
s)?Te(L)?NbTe4(s) that takes place at 465 °C had its
isothermal transformation line extended from 75 to 66.67
at.% Te, becoming NbTe2(s)?Te(L)?NbTe4(s). Another
valid hypothesis is that NbTe2 (C2/m) experiment an
enlargement of the composition range of NbTe2 towards
the Te rich compositions over 500 °C. In other words,
monoclinic NbTe2 (C2/m) is formed before the reaction
takes place during cooling. Hence, the relative amount of
this phase in samples treated at 500 °C should be higher.
Also, the fact that the samples prepared at 400 °C did not
show any trace of the phases Nb3Te7, Nb3Te8 and NbTe3 is
strong experimental evidence that supports this claim. By
assuming that this is true, the rapid cooling from the
quenching procedure would develop a microstructure that
is richer in NbTe2.
4.3 Phase Transformations
In order to investigate the phase reactions that would form
Nb5Te4 and Nb3Te4, Differential Thermal Analysis mea-
surements were carried out with portions of samples # 20 to
# 22 taken after the annealing process. These results are
shown in Fig. 7. The transition temperatures were
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702 J. Phase Equilib. Diffus. (2019) 40:697–705

Fig. 5 SEM BSE micrographs

of samples (a) # 13, (b) # 14,
(c) # 16 and (d) # 19

Fig. 6 XRD data of samples # 20 to # 26 with nominal composition

varying from 44.4 to 80 at.% Te heat-treated at 500 °C for 744 h

determined as the onset temperature of the observed tran-

sition. This criterion was applied first in sample # 22 (lower
panel of Fig. 7). Sample # 22 is, among these three sam-
ples, the only that exhibits tetragonal NbTe4 in its
microstructure. Also, thermogravimetric analysis shows a
significant mass loss for this sample (data not shown). At
1200 °C, the remaining mass was 35% of the initial mass,
which suggests the formation of a Te-rich liquid phase. The
Fig. 7 Differential thermal analysis data of the samples # 20, # 21,
and # 22
Te vaporization in this liquid is largely promoted too due to
its high chemical activity. Therefore, these results suggest
that the transition observed at 443 °C should be related to
the transformation of NbTe4. The DTA data of sample # 22
did not show any transition in the vicinity of 465 °C,

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J. Phase Equilib. Diffus. (2019) 40:697–705
suggesting that the temperature of the transformation
between Te(L) and NbTe2 transition should occur at lower
temperatures. Considering the melting point of pure Te as
449.5 °C, it requires two pairs of invariant reactions to
satisfy the phase rules for NbTe4 and Te(L): (1) NbTe2-
? Te(L) ? NbTe4 and Te(L) ? NbTe4 ?TeSS, or (2)
Te(L) ? NbTe2 ?TeSS and NbTe2 ? TeSS ? NbTe4
assuming that the solubility of Nb in TeSS is smaller than in
Te(L). Both scenarios may be proposed, considering that
the temperatures of these transitions are in the vicinity of
the melting point of pure Te. More experimental work
focused on this region of the phase diagram is necessary to
propose accurate reactions between these phases.
Concerning the data from samples # 20 and # 21, two
transitions are observed. The first one in the vicinity of
735 °C (we have adopted the onset temperature on heating
to define the transition temperature) and the second one in
the vicinity of 839 °C. The formation energy for Nb5Te4
(I4/m) and Nb3Te4 (P63/m) calculated using the general-
ized gradient approximation are - 0.356 and - 0.458 eV/
atom respectively,[32] Given the fact that Nb3Te4 is actually
a ground state according to Ref 32, and Nb5Te4 is just
above the convex hull one would expect Nb3Te4 to be
stable to lower temperatures. At low temperatures, a mix-
ture of Nb ? Nb3Te4 is more stable than Nb5Te4 because
with increasing temperature Nb5Te4 is stabilized by having
a larger entropy than the Nb ? Nb3Te4 mixture. Taking
into account these arguments, the transitions observed can
be associated with the following eutectoid reactions:
At 735 °C:
Fig. 8 Proposed Nb-Te binary
phases diagram
703
Nb3 Te4ðsÞ ! Nbss þ NbTe2ðsÞ ðEq 1Þ
At 839 °C:
Nb5 Te4ðsÞ ! Nbss þ Nb3 Te4ðsÞ ðEq 2Þ
5 Summary
The binary Nb-Te phase diagram was investigated. Results
of XRD demonstrate that the Nb-rich side of the phase
diagram is composed of a two-phase region of NbSS and
Nb5Te4 (I4/m). Furthermore, a careful investigation was
carried out in the Te-rich side of the phase diagram at 400
and 500 °C. Results of XRD data and SEM micrographs
show that, at this temperature range, the only stable inter-
metallic phases are NbTe2 (C2/m) and NbTe4 (P4/mcc).
DTA measurements show endothermic transitions at
443 , at 735 and 839 °C. The transition observed at
443 °C is related to NbTe4 and Te(L). Considering the
melting point of pure Te as 449.5 °C, it requires two pairs
of invariant reactions to satisfy the phase rule: (1) NbTe2-
? Te(L) ? NbTe4 and Te(L) ? NbTe4 ?TeSS, or (2)
Te(L) ? NbTe2 ? TeSS and NbTe2 ? TeSS ? NbTe4
assuming that the solubility of Nb in TeSS is smaller than in
Te(L). Generalized gradient approximation calculation of
the formation energy of Nb3Te4 and Nb5Te4 suggest that
the two high-temperature transitions observed at 735 and
839 °C are related to the eutectoid decomposition of Nb3-
Te4 (P63/m) and Nb5Te4 (I4/m) respectively. Figure 8
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presents a proposal for the binary Nb-Te phase diagram
constructed based on the results obtained in this work.
6 Conclusions
This report studied the binary Nb-Te phase diagram. X-ray
diffraction, Rietveld refinement, and SEM micrographs
show that monoclinic NbTe2 (C2/m) and tetragonal NbTe4
(P4/mcc) are the only stable intermetallic phases in the Te
rich side of this system at low temperatures. Differential
thermal analysis data suggest that the transition observed at
443 °C is related to reactions between NbTe2, NbTe4 and
Te(L). From the literature, generalized gradient approxi-
mation of the formation energy of Nb3Te4 and Nb5Te4
suggest that a mixture of Nb ? Nb3Te4 is more stable than
Nb5Te4, which indicates that the transitions observed at
735 and 839 °C are related to the peritectic transformation
of Nb3Te4 (P63/m) and Nb5Te4 (I4/m) respectively. The
results presented in this report open path to new experi-
mental studies on the high-temperature region and liquid
phase of the Nb-Te system and are helpful for thermody-
namic modeling of this system.
Acknowledgments This report is based upon financial support by the
Brazilian research agencies CAPES, CNPq (302850/2014-7,
443385/2014-9, and 142016/2013-6) and FAPESP (2013/16873-3).
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