X-ray absorption near edge spectroscopy of thermochromic phase transition in CuMoO₄
Thermochromic phase transition was studied in CuMoO₄ using the Cu and Mo K-edge x-ray absorption spectroscopy in the temperature range of 10–300 K. The hysteretic behavior has been evidenced from the temperature dependence of the pre-edge shoulder intensity at the Mo K-edge, indicating that the tran...
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irk-123456789-1761192021-02-04T01:28:58Z X-ray absorption near edge spectroscopy of thermochromic phase transition in CuMoO₄ Jonane, I. Cintins, A. Kalinko, A. Chernikov, R. Kuzmin, A. Динамика кристаллической решетки Thermochromic phase transition was studied in CuMoO₄ using the Cu and Mo K-edge x-ray absorption spectroscopy in the temperature range of 10–300 K. The hysteretic behavior has been evidenced from the temperature dependence of the pre-edge shoulder intensity at the Mo K-edge, indicating that the transition from brownish-red γ-CuMoO₄ to green α-CuMoO₄ occurs in the temperature range of 230–280 K upon heating, whereas the α-to-γ transition occurs between 200 and 120 K upon cooling. Such behavior of the pre-edge shoulder at the Mo K-edge correlates with the change of molybdenum coordination between distorted tetrahedral in α-CuMoO₄ and distorted octahedral in γ-CuMoO₄. This result has been supported by ab initio full-multiple-scattering x-ray absorption near edge structure (XANES) calculations. 2018 Article X-ray absorption near edge spectroscopy of thermochromic phase transition in CuMoO₄ / I. Jonane, A. Cintins, A. Kalinko, R. Chernikov, A. Kuzmin // Физика низких температур. — 2018. — Т. 44, № 5. — С. 568-572. — Бібліогр.: 39 назв. — англ. 0132-6414 PACS: 61.05.cj, 64.70.kp http://dspace.nbuv.gov.ua/handle/123456789/176119 en Физика низких температур Фізико-технічний інститут низьких температур ім. Б.І. Вєркіна НАН України |
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Динамика кристаллической решетки Динамика кристаллической решетки |
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Динамика кристаллической решетки Динамика кристаллической решетки Jonane, I. Cintins, A. Kalinko, A. Chernikov, R. Kuzmin, A. X-ray absorption near edge spectroscopy of thermochromic phase transition in CuMoO₄ Физика низких температур |
| description |
Thermochromic phase transition was studied in CuMoO₄ using the Cu and Mo K-edge x-ray absorption spectroscopy in the temperature range of 10–300 K. The hysteretic behavior has been evidenced from the temperature dependence of the pre-edge shoulder intensity at the Mo K-edge, indicating that the transition from brownish-red γ-CuMoO₄ to green α-CuMoO₄ occurs in the temperature range of 230–280 K upon heating, whereas the α-to-γ transition occurs between 200 and 120 K upon cooling. Such behavior of the pre-edge shoulder at the Mo K-edge correlates with the change of molybdenum coordination between distorted tetrahedral in α-CuMoO₄ and distorted octahedral in γ-CuMoO₄. This result has been supported by ab initio full-multiple-scattering x-ray absorption near edge structure (XANES) calculations. |
| format |
Article |
| author |
Jonane, I. Cintins, A. Kalinko, A. Chernikov, R. Kuzmin, A. |
| author_facet |
Jonane, I. Cintins, A. Kalinko, A. Chernikov, R. Kuzmin, A. |
| author_sort |
Jonane, I. |
| title |
X-ray absorption near edge spectroscopy of thermochromic phase transition in CuMoO₄ |
| title_short |
X-ray absorption near edge spectroscopy of thermochromic phase transition in CuMoO₄ |
| title_full |
X-ray absorption near edge spectroscopy of thermochromic phase transition in CuMoO₄ |
| title_fullStr |
X-ray absorption near edge spectroscopy of thermochromic phase transition in CuMoO₄ |
| title_full_unstemmed |
X-ray absorption near edge spectroscopy of thermochromic phase transition in CuMoO₄ |
| title_sort |
x-ray absorption near edge spectroscopy of thermochromic phase transition in cumoo₄ |
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Фізико-технічний інститут низьких температур ім. Б.І. Вєркіна НАН України |
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2018 |
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Динамика кристаллической решетки |
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http://dspace.nbuv.gov.ua/handle/123456789/176119 |
| citation_txt |
X-ray absorption near edge spectroscopy of thermochromic phase transition in CuMoO₄ / I. Jonane, A. Cintins, A. Kalinko, R. Chernikov, A. Kuzmin // Физика низких температур. — 2018. — Т. 44, № 5. — С. 568-572. — Бібліогр.: 39 назв. — англ. |
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Физика низких температур |
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| fulltext |
Low Temperature Physics/Fizika Nizkikh Temperatur, 2018, v. 44, No. 5, pp. 568–572
X-ray absorption near edge spectroscopy
of thermochromic phase transition in CuMoO4
I. Jonane1, A. Cintins1, A. Kalinko2, R. Chernikov3, and A. Kuzmin1
1Institute of Solid State Physics, University of Latvia, 8 Kengaraga Str., Riga LV-1063, Latvia
E-mail: inga.jonane@cfi.lu.lv
2Universität Paderborn, Naturwissenschaftliche Fakultät, Department Chemie,
100 Warburger Str., Paderborn 33098, Germany
3DESY Photon Science, 85 Notkestraße, Hamburg D-22607, Germany
Received October 26, 2017, published online March 27, 2018
Thermochromic phase transition was studied in CuMoO4 using the Cu and Mo K-edge x-ray absorption spec-
troscopy in the temperature range of 10–300 K. The hysteretic behavior has been evidenced from the tempera-
ture dependence of the pre-edge shoulder intensity at the Mo K-edge, indicating that the transition from brown-
ish-red γ-CuMoO4 to green α-CuMoO4 occurs in the temperature range of 230–280 K upon heating, whereas the
α-to-γ transition occurs between 200 and 120 K upon cooling. Such behavior of the pre-edge shoulder at the Mo
K-edge correlates with the change of molybdenum coordination between distorted tetrahedral in α-CuMoO4 and
distorted octahedral in γ-CuMoO4. This result has been supported by ab initio full-multiple-scattering x-ray ab-
sorption near edge structure (XANES) calculations.
PACS: 61.05.cj X-ray absorption spectroscopy: EXAFS, NEXAFS, XANES, etc.;
64.70.kp Ionic crystals.
Keywords: x-ray absorption spectroscopy, CuMoO4, thermochromism, phase transition.
Introduction
Molybdates and tungstates find a wide range of practi-
cal applications due to their ability to adopt different crys-
tallographic structures, whose physical properties can be
further modified by a chemical composition [1,2]. In par-
ticular, these materials are used as scintillators, down-
conversion phosphors, white light-emitting diodes, laser
host materials, catalysts, sensors and pigments [3–12].
Copper molybdate CuMoO4 is a functional oxide material
exhibiting thermochromic and piezochromic properties [13–
15]. It attracts much attention because of its potential applica-
tions for temperature sensing in the ranges where majority of
organic compounds and liquid crystals are unstable. Possible
chromic-related applications extend from the user-friendly
temperature and pressure indicators [14–17] to “smart” inor-
ganic pigments [18]. Besides, copper molybdate has also
promising catalytic properties [19–23].
Structural, optical, electrical and magnetic properties
of CuMoO4 were previously studied in [13,24–27]. Cur-
rently six different structural phases of CuMoO4 are
known [24,28]. In this study, we focus on two of them —
green α-CuMoO4 and brownish-red γ-CuMoO4 phases
that are stable at high and low temperatures, respectively
(Fig. 1).
At ambient pressure and room temperature, CuMoO4 has
α-phase with triclinic structure (space group P-1) [24,29]. It
is composed of distorted CuO6 octahedra, CuO5 square-
pyramids and MoO4 tetrahedra. By decreasing temperature
below ∼200 K (or by applying pressure above 0.2 GPa at
Fig. 1. (Color online) Crystalline structures of high-temperature α-
CuMoO4 and low-temperature γ-CuMoO4 phases [24].
© I. Jonane, A. Cintins, A. Kalinko, R. Chernikov, and A. Kuzmin, 2018
X-ray absorption near edge spectroscopy of thermochromic phase transition in CuMoO4
room temperature) reversible first order phase transition from
α-CuMoO4 to γ-CuMoO4 occurs [24]. Low-temperature γ
modification also has triclinic lattice (space group P-1) built
up of distorted CuO6 and MoO6 octahedra [25]. The α-to-γ
phase transition is accompanied by color change (from green
to brownish-red) and volume reduction of 12–13% [24] that
makes the two phases easily distinguishable. However, the
presence in both phases of three non-equivalent Cu and Mo
atoms with different local environment makes structural
analysis challenging [24].
The α-to-γ phase transition occurring below room tem-
perature was studied previously using x-ray diffraction
[24] and optical spectroscopy [14,26], differential scanning
calorimetry and magnetic susceptibility [14] measure-
ments. It was found that the transition has hysteretic be-
havior, so that lower temperature is required to promote
the α-to-γ transition than γ-to-α.
Chromic properties of CuMoO4 are associated with the
interplay between two optical absorption bands: the one in
the blue range (around 3 eV) is due to the interband transi-
tion across the band gap of the crystal and the second one
in the red (around 1.49 eV) originates due to the intraband
d-d transition at copper [13,14,26]. Note that the thermo-
chromic phase transition is strongly affected by chemical
composition: for example, an addition of tungsten to
CuMoO4 results in a formation of solid solutions
CuMo1−xWxO4 (x ≤ 0.12) and shifts the transition tempera-
ture by up to 100 K [14,18,24].
Since thermochromic and piezochromic properties of
CuMoO4 are connected with its local structure, x-ray ab-
sorption spectroscopy (XAS) is an obvious choice to probe
structural changes during the phase transition. XAS pro-
vides information complementary to other techniques and,
in the case of CuMoO4 can probe the local environment
around Cu and Mo atoms independently by detecting two
different absorption edges. Therefore, we have performed
the temperature-dependent (10–300 K) Cu and Mo K-edge
XAS study of thermochromic phase transition in CuMoO4
at the new P65 beamline (HASYLAB at DESY, Hamburg)
using the synchrotron radiation from the PETRA-III stor-
age ring. The obtained results allowed us to confirm the
hysteretic nature of phase transition and to explain the in-
fluence of structural changes on the x-ray absorption near
edge structure based on ab initio full-multiple-scattering
calculations.
Experimental and data analysis
Polycrystalline CuMoO4 powder was synthesized using
solid-state reaction method by heating a mixture of CuO
and MoO3 powders at 650 °C in air for 8 h followed by
cooling down to room temperature. The as-prepared pow-
der corresponded to α-CuMoO4 phase and had green color.
Temperature-dependent (from 10 to 300 K) x-ray absorp-
tion experiments were conducted at the HASYLAB PETRA-
III P65 undulator beamline. The PETRA-III storage ring
operated at E = 6.08 GeV and current I = 95 mA in top-up
40 bunch mode. The harmonic rejection was achieved by
uncoated (Cu edge) and Rh-coated (Mo edge) silicon plane
mirrors. Fixed exit Si(311) double-crystal monochromator
was used in all experiments. The x-ray absorption spectra
were collected at the Cu (8979 eV) and Mo (20000 eV)
K-edges in transmission mode using two ionization
chambers. The Oxford Instruments liquid helium flow
cryostat was used to maintain the sample temperature.
The CuMoO4 powder was gently milled in agate mortar
and deposited on Millipore membrane.
The Cu and Mo K-edge XANES parts of the x-ray ab-
sorption spectra were isolated and used in the further analy-
sis. It was observed that the Cu K-edge XANES spectra do
not vary significantly upon temperature change indicating
some stability of the copper environment. Therefore, they
will not be discussed further. At the same time, the Mo
K-edge XANES was significantly affected by temperature
variation. The experimental Mo and Cu K-edge XANES
spectra corresponding to γ-CuMoO4 at 10 K and α-CuMoO4
at 300 K are shown in Figs. 2(a),(b). The pre-edge shoulder
at the Mo K-edge is clearly visible around 20000 eV, and its
change can be related to a transition from MoO4 tetrahedra
to MoO6 octahedra upon cooling. At the same time, the Cu
K-edge XANES does not change significantly upon phase
transition.
A fraction of α-CuMoO4 phase was evaluated at each
temperature during heating from 10 to 300 K and cooling
from 300 down to 100 K using a linear combination of
the lowest temperature (10 K) and highest temperature
(300 K) Mo K-edge XANES. The analysis was performed
using Athena package [30] in the energy range from
19980 to 20010 eV with the aim to sample a variation of
the pre-edge shoulder. The obtained results are shown in
Fig. 3, where the hysteretic behavior is well observed.
XANES calculations
Full-multiple-scattering (FMS) XANES calculations
were performed using ab initio real-space FDMNES code
[31,32] employing muffin-tin (10% overlap) self-consistent
potential. The dipole and quadrupole transitions were taken
into account, and the energy-dependent real Hedin–
Lundqvist exchange-correlation potential was used [33,34].
The calculated XANES spectra were broadened to account
for the core-hole level width (5.8 eV at the Mo K-edge [35])
and other multielectronic phenomena. The energy origin was
set at the Fermi level EF.
The results of FMS XANES calculations for five MoOx
clusters are shown in Fig. 2(c). They correspond to regular
MoO4 tetrahedron (R(Mo–O) = 1.78 Å), regular MoO6
octahedron (R(Mo–O) = 1.98 Å) and distorted MoO6
octahedra with molybdenum ion being displaced in the
direction of octahedron apex by 0.2 Å (<100>), to the oc-
Low Temperature Physics/Fizika Nizkikh Temperatur, 2018, v. 44, No. 5 569
I. Jonane, A. Cintins, A. Kalinko, R. Chernikov, and A. Kuzmin
tahedron edge by 0.28 Å (〈110〉) and to the octahedron face
by 0.35 Å (〈111〉).
FMS XANES calculations were also performed for α-
and γ-CuMoO4 structural models created using diffraction
data from [24]. The total calculated Mo K-edge XANES
spectra and separate contributions from non-equivalent
molybdenum atoms (Mo1, Mo2 and Mo3) are compared
with the experimental data in Fig. 4.
Results and discussion
The Mo K-edge XANES spectra of CuMoO4 at two
temperatures (10 and 300 K) are shown in Fig. 2(a). The
pre-edge shoulder at ∼20000 eV corresponds to the
1s(Mo) → 4d(Mo) + 2p(O) transition. Note that the final
state of the electron is the relaxed excited state in the pres-
ence of the core hole at the 1s(Mo) level screened by other
electrons. The transition is forbidden in the dipole approx-
imation for a regular MoO6 octahedron, having an inver-
sion center, but becomes allowed when inversion sym-
metry is broken as in distorted octahedron [36,37] or in
tetrahedron [38] (Fig. 2(c)). The amplitude of the pre-edge
shoulder depends on the degree of the MoO6 octahedra
distortion and 4d(Mo)/2p(O) orbital mixing and is the larg-
est for tetrahedral MoO4 coordination [39]. Therefore, it
can be used to monitor the γ-to-α phase transition in
CuMoO4.
Since accurate separation of the pre-edge shoulder from
the main absorption edge is tricky, we employed a different
approach: the experimental XANES spectrum at each tem-
perature was approximated by a linear combination of the
lowest temperature (10 K) and highest temperature (300 K)
XANES spectra. As a result, the fraction of the α-CuMoO4
phase in the total XANES upon heating and cooling was
estimated and is reported in Fig. 3. As one can see, only
γ-CuMoO4 is present below 150 K and only α-CuMoO4
is observed above 280 K, as expected.
Linear combination analysis showed that upon heating,
the γ-to-α phase transition occurs between ∼230–280 K,
whereas upon cooling, the α-to-γ transition takes place at
lower temperature between ∼120–200 K, showing a large
hysteresis loop with the range of two phase coexistence of
about 50–80 K. Following the notation from [14], two tem-
perature T1/2H and T1/2C corresponding to about 50 mol% of
the α and γ phases upon heating and cooling, respectively,
are equal to T1/2H ≈ 255 K and T1/2C ≈ 143 K. The width of
the hysteresis is defined as ∆T1/2C = T1/2C − T1/2H = 112 K.
Fig. 2. (Color online) (a),(b) Experimental Mo and Cu K-edge
XANES of α-CuMoO4 (at 300 K) and γ-CuMoO4 (at 10 K)
phases. (c) Calculated Mo K-edge XANES for regular MoO4
tetrahedron, distorted and regular MoO6 octahedra. Numbers in
brackets indicate the direction of molybdenum ion off-center
displacement. See text for more details.
Fig. 3. Temperature dependence of the fraction of α-CuMoO4
phase upon heating (solid circles) and cooling (open circles).
570 Low Temperature Physics/Fizika Nizkikh Temperatur, 2018, v. 44, No. 5
X-ray absorption near edge spectroscopy of thermochromic phase transition in CuMoO4
Note that our value of ∆T1/2 is slightly larger than those es-
timated from optical reflectivity (∆T1/2 = 72 K), differential
scanning calorimetry (∆T1/2 = 96 K) and magnetic suscepti-
bility (∆T1/2 = 80 K) measurements in [14].
FMS Mo K-edge XANES calculations performed for
α-CuMoO4 and γ-CuMoO4 phases are shown in Fig. 4.
They are in a reasonable agreement with the experimental
data. Since there are three non-equivalent molybdenum
atoms in the unit cells of both molybdates [24], we have
calculated also their contributions into the total XANES
spectrum (see two lower panels in Fig. 4).
As one can see, the three molybdenum atoms, located in
distorted tetrahedral coordination with the Mo–O distances
ranged between 1.70 and 1.86 Å [24], produce slightly dif-
ferent XANES for α-CuMoO4. At the same time, the three
contributions to XANES from molybdenum atoms, located
in strongly distorted octahedral environment with the Mo–O
bond lengths ranged between 1.68 and 2.49 Å [24], are close
for γ-CuMoO4, except for the region of the pre-edge peak.
These differences are caused by an influence of outer coor-
dination shells located above 2.5 Å, whose detailed analysis
using reverse Monte Carlo approach is in progress.
Conclusions
We report the first in situ x-ray absorption spectrosco-
py study of the thermochromic phase transition between
brownish-red γ-CuMoO4 and green α-CuMoO4 in the
temperature range from 10 to 300 K. We found that the
Cu K-edge XANES is weakly affected upon the phase
transition because the local environment of copper atoms
does not change significantly. At the same time, the anal-
ysis of the Mo K-edge XANES allowed us to follow the
transition, tracing a variation of the pre-edge shoulder.
The experimental Mo K-edge XANES data were inter-
preted based on ab initio full-multiple-scattering calcula-
tions. Good agreement was found between the experi-
mental and simulated XANES spectra, and the contribution
from non-equivalent molybdenum atoms in the crystal-
lographic unit cell was estimated. It was shown that the
amplitude of the pre-edge shoulder correlates with the type
and the degree of distortion of molybdenum–oxygen coor-
dination polyhedra.
A significant variation of the experimental Mo K-edge
XANES upon the thermochromic transition occurs due to
the change of the local environment of molybdenum atoms
from distorted tetrahedral in green α-CuMoO4 to distorted
octahedral in brownish-red γ-CuMoO4. Moreover, the
thermochromic transition has well evidenced hysteretic be-
havior, in agreement with the results of previous studies
[14]. The transition from the γ-to-α phase occurs in the tem-
perature range of 230–280 K upon heating, whereas the α-
to-γ transition occurs between 120 and 200 K upon cooling.
The width of the hysteresis was estimated to be about 112 K.
Acknowledgments
Financial support provided by Scientific Research Project
for Students and Young Researchers Nr. SJZ/2017/5 realized
at the Institute of Solid State Physics, University of Latvia is
greatly acknowledged. The experiment at HASYLAB/DESY
was performed within the project I-20160149 EC.
Fig. 4. (Color online) Comparison of the experimental and calcu-
lated Mo K-edge XANES of α-CuMoO4 and γ-CuMoO4 phases
(upper panel). Contributions from three non-equivalent molyb-
denum atoms (Mo1, Mo2, Mo3) to the Mo K-edge XANES are
also shown in the middle and lower panels for α-CuMoO4 and
γ-CuMoO4 phases, respectively.
Low Temperature Physics/Fizika Nizkikh Temperatur, 2018, v. 44, No. 5 571
I. Jonane, A. Cintins, A. Kalinko, R. Chernikov, and A. Kuzmin
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Introduction
Experimental and data analysis
XANES calculations
Results and discussion
Conclusions
Acknowledgments
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