Formation of nanostructured state in LaBGeO₅ monolithic glass using pulsed magnetic fields
Using the methods of transmission electron microscopy, X-ray structure analysis and thermal differential analysis, it has been discovered that the pulsed magnetic field (PMF) intensifies homogeneous crystallization in LaBGeO₅-glass system, promotes homogenization of crystalline phase distribution in...
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Інститут фізики напівпровідників імені В.Є. Лашкарьова НАН України
2016
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| Цитувати: | Formation of nanostructured state in LaBGeO₅ monolithic glass using pulsed magnetic fields / A.S. Doroshkevich, A.V. Shylo, G.K. Volkova, V.A. Glazunova, L.D. Perekrestova, S.B. Lyubchik, T.E. Konstantinova // Semiconductor Physics Quantum Electronics & Optoelectronics. — 2016. — Т. 19, № 3. — С. 267-272. — Бібліогр.: 23 назв. — англ. |
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irk-123456789-1215982017-06-15T03:05:48Z Formation of nanostructured state in LaBGeO₅ monolithic glass using pulsed magnetic fields Doroshkevich, A.S. Shylo, A.V. Volkova, G.K. Glazunova, V.A. Perekrestova, L.D. Lyubchik, S.B. Konstantinova, T.E. Using the methods of transmission electron microscopy, X-ray structure analysis and thermal differential analysis, it has been discovered that the pulsed magnetic field (PMF) intensifies homogeneous crystallization in LaBGeO₅-glass system, promotes homogenization of crystalline phase distribution inside the bulk of glass matrix. A possibility of obtaining the volume nanostructured state in LaBGeO₅-glass due to application of PMF has been suggested and experimentally grounded. 2016 Article Formation of nanostructured state in LaBGeO₅ monolithic glass using pulsed magnetic fields / A.S. Doroshkevich, A.V. Shylo, G.K. Volkova, V.A. Glazunova, L.D. Perekrestova, S.B. Lyubchik, T.E. Konstantinova // Semiconductor Physics Quantum Electronics & Optoelectronics. — 2016. — Т. 19, № 3. — С. 267-272. — Бібліогр.: 23 назв. — англ. 1560-8034 DOI: 10.15407/spqeo19.03.267 PACS 65.60.+a, 68.35.Rh http://dspace.nbuv.gov.ua/handle/123456789/121598 en Semiconductor Physics Quantum Electronics & Optoelectronics Інститут фізики напівпровідників імені В.Є. Лашкарьова НАН України |
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Digital Library of Periodicals of National Academy of Sciences of Ukraine |
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Using the methods of transmission electron microscopy, X-ray structure analysis and thermal differential analysis, it has been discovered that the pulsed magnetic field (PMF) intensifies homogeneous crystallization in LaBGeO₅-glass system, promotes homogenization of crystalline phase distribution inside the bulk of glass matrix. A possibility of obtaining the volume nanostructured state in LaBGeO₅-glass due to application of PMF has been suggested and experimentally grounded. |
| format |
Article |
| author |
Doroshkevich, A.S. Shylo, A.V. Volkova, G.K. Glazunova, V.A. Perekrestova, L.D. Lyubchik, S.B. Konstantinova, T.E. |
| spellingShingle |
Doroshkevich, A.S. Shylo, A.V. Volkova, G.K. Glazunova, V.A. Perekrestova, L.D. Lyubchik, S.B. Konstantinova, T.E. Formation of nanostructured state in LaBGeO₅ monolithic glass using pulsed magnetic fields Semiconductor Physics Quantum Electronics & Optoelectronics |
| author_facet |
Doroshkevich, A.S. Shylo, A.V. Volkova, G.K. Glazunova, V.A. Perekrestova, L.D. Lyubchik, S.B. Konstantinova, T.E. |
| author_sort |
Doroshkevich, A.S. |
| title |
Formation of nanostructured state in LaBGeO₅ monolithic glass using pulsed magnetic fields |
| title_short |
Formation of nanostructured state in LaBGeO₅ monolithic glass using pulsed magnetic fields |
| title_full |
Formation of nanostructured state in LaBGeO₅ monolithic glass using pulsed magnetic fields |
| title_fullStr |
Formation of nanostructured state in LaBGeO₅ monolithic glass using pulsed magnetic fields |
| title_full_unstemmed |
Formation of nanostructured state in LaBGeO₅ monolithic glass using pulsed magnetic fields |
| title_sort |
formation of nanostructured state in labgeo₅ monolithic glass using pulsed magnetic fields |
| publisher |
Інститут фізики напівпровідників імені В.Є. Лашкарьова НАН України |
| publishDate |
2016 |
| url |
http://dspace.nbuv.gov.ua/handle/123456789/121598 |
| citation_txt |
Formation of nanostructured state in LaBGeO₅ monolithic glass using pulsed magnetic fields / A.S. Doroshkevich, A.V. Shylo, G.K. Volkova, V.A. Glazunova, L.D. Perekrestova, S.B. Lyubchik, T.E. Konstantinova // Semiconductor Physics Quantum Electronics & Optoelectronics. — 2016. — Т. 19, № 3. — С. 267-272. — Бібліогр.: 23 назв. — англ. |
| series |
Semiconductor Physics Quantum Electronics & Optoelectronics |
| work_keys_str_mv |
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2025-07-08T20:11:49Z |
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2025-07-08T20:11:49Z |
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| fulltext |
Semiconductor Physics, Quantum Electronics & Optoelectronics, 2016. V. 19, N 3. P. 267-272.
doi: 10.15407/spqeo19.03.267
© 2016, V. Lashkaryov Institute of Semiconductor Physics, National Academy of Sciences of Ukraine
267
PACS 65.60.+a, 68.35.Rh
Formation of nanostructured state in LaBGeO5 monolithic glass
using pulsed magnetic fields
A.S. Doroshkevich1,2, A.V. Shylo2, G.K. Volkova3, V.A. Glazunova3, L.D. Perekrestova2,
S.B. Lyubchik4, T.E. Konstantinova2
1Joint Institute for Nuclear Research, Joliot-Curie str., 6, Dubna, 141980, Russia
2Donetsk Institute for Physics and Engineering, NAS of Ukraine,
46, Nauki ave, 03083 Kyiv, Ukraine
3Government institution “Donetsk Institute for Physics and Engineering”,
72, R. Luksemburg str. Donetsk, 83114, Ukraine
4REQUIMTE, Universidade Nova de Lisboa, 2829-516, Caparica, Portugal
Correspondence author e-mail: doroh@jinr.ru
Abstract. Using the methods of transmission electron microscopy, X-ray structure
analysis and thermal differential analysis, it has been discovered that the pulsed magnetic
field (PMF) intensifies homogeneous crystallization in LaBGeO5-glass system, promotes
homogenization of crystalline phase distribution inside the bulk of glass matrix. A
possibility of obtaining the volume nanostructured state in LaBGeO5-glass due to
application of PMF has been suggested and experimentally grounded.
Keywords: glass nanocomposites, sensors, stillwellite, pulsed magnetic field.
Manuscript received 13.04.16; revised version received 14.07.16; accepted for
publication 13.09.16; published online 04.10.16.
1. Introduction
Development of optoelectronics, photonics and
communication technologies has greatly increased
demand for novel advanced materials with non-linear
optical or sensor (pyroelectric, ferroelectric, etc.)
properties. In this relation, glass is of great interest as a
class of the materials that combines extremely high
optical performance and low-cost as compared with
monocrystalline analogues.
In the past, glass was considered as a viscous liquid
with short-range order, while crystalline matter was
attributed to the presence both short– and long-range
orders [1, 2]. Nowadays, the crystalline and amorphous
states are no longer regarded as strictly polar substance
of the condensed matter. For instance, intermediate
nanoscale states were found in solid solutions of glass at
initial stages of phase separation, which are responsible
for unique combination of electrical, mechanical and
optical properties [3]. Controlled formation of the glass
functional structures at nanoscale is extremely
perspective for a new generation of the functional
materials, such as transparent ferroelectric glass ceramic,
glass with piezo- and pyroelectric properties, gradient
optical media for laser technologies, optoelectronics and
photonics.
Ferroelectric LaBGeO5-glass (LBG) along with
unique combination of pyroelectric properties, like low
ferroelectric losses (tg δ ~ 0.001) at a significant level of
pyroelectric activity (γ ~ 5…10 nC/cm2K), high value of
electrical resistance (ρv > 10 GOhm·cm at 300 K) [4, 5],
high coercive force and ability to bulk polarization, has
Semiconductor Physics, Quantum Electronics & Optoelectronics, 2016. V. 19, N 3. P. 267-272.
doi: 10.15407/spqeo19.03.267
© 2016, V. Lashkaryov Institute of Semiconductor Physics, National Academy of Sciences of Ukraine
268
the coefficient of thermal expansion (CTE) of (6×10–
6)K–1 [6], which corresponds to the ceramic materials.
Therefore, due to nanostructural organization, the
composite materials based on LaBGeO5-glass are
promising for usage both as an active media for lasers
and optoelectronic communication technologies
(namely, for active elements of generating, amplifying
and controlling systems) as well as a constructural
material for high-temperature ceramic composites in the
solid oxide fuel cell technology (SOFC).
Due to superficial nature of LBG-glass
crystallization, it is very difficult to get a high dense,
nanodimensional crystalline phase in a bulk, which is
responsible for functional and physical-mechanical
properties of the resulted materials.
Taking into account the significant thermodynamic
instability of the glass structure and quantum nature of
the nanosized crystalline cells formation process in the
bulk of a glass matrix, one of the promising approaches
is usage of an external structure-forming actions of
electromagnetic nature, namely, pulsed magnetic fields
(PMF).
It was shown for a wide range of non-magnetic
materials that PMF initiates a long-term change of the
structure and physical properties in condensed matter.
Both melting temperature, activation energy and
crystallization temperature changed after brief exposure
by weak PMF of 105…106 A/m [7, 8, 9]. However, the
questions of the nanoscale structures formation in oxide
glass using PMF are not enough highlighted in literature.
The possibility of weak PMF to intensify the processes
of structural transformation in oxide glass, in particular
of MgO-Al2O3-SiO2 composition [10], and bulk
character of the electromagnetic field influence on
diamagnetic materials allows to expect a positive PMF
effect on nanostructures formation in LBG-glass.
This work is aimed at validation of the above
mentioned statement and investigation of the relevant
effects of weak PMF influence on structural
transformation in the bulk of LBG glass system.
2. Experimental
Amorphous glass was obtained by fast cooling between
metal plates, the mixture consisted of molten oxides of
LaO2 (25%) – 50B2O3 (50%) – 25GeO5 (25%). The melt
was obtained by induction heating of the co-mingled
oxides up to a 1500 °C in a platinum crucible and
soaking time of 20 min. After polishing, the transparent
LaBGeO5-glass plates (with the surface area close to
1 cm2 and the average weight of 0.6 g) were subjected to
the thermal treatment at 600 °C for 2 h aimed at removal
of internal stresses. The obtained samples were treated at
room temperature by exponentially growing weak
magnetic field pulses (peak intensity (H) of 106 A/m)
with the frequency (f) close to 1 Hz, while the untreated
ones were used as reference onset. Then, the
crystallization annealing of the samples was performed
in two steps: (1) “step-by-step” increase of temperature
for 6 h between 650 tо 680 °С with the step of 5 °С;
followed by (2) increase of the temperature up to 705 °С
and soaking time 2 h.
In some cases, PMF treatment was carried out both
at room temperature and at annealing stage as well.
Samples were studied using X-ray analysis (XRD) with
DRON-3 diffractometer, Electron Spin Resonance
(ESR) with RE-1306 spectrometer, Differential Thermal
Analysis (DTA) with “Metler” derivatograph, Optical
(POLAM R-311 polarization microscope) and
Transmission Electron Microscopy (TEM) with JEM
200A devices. Before registering the ESR spectra, the
reference and PMF-treated samples were subjected to
the thermal treatment at 530 °С for 2 h and then exposed
by strong X-ray radiation for 45 min at room
temperature.
3. Results and discussion
According to X-ray investigation, the LaBGeO5 crystal
has monoclinic structure1) and belongs to the simple
monocentric compounds (acentric spatial groups of P31
or P3121) [11]. The stillwellite structure consists of
spiral positioned chains of BO4 tetrahedrons, (B–O
bonds are of 1.454…1.502 Å), which stretches along the
helical axis of the third order (Fig. 1a). In the LaBGeO5
structures, atoms of Ge are similar to Si atoms in
LaBSiO5 stillwellite and are arranged in distorted
tetrahedrons (Ge–O bonds are of 1.719…1.789 Å), La
atoms are arranged in 9-hedrons (polyhedrons) above
and under the Ge-tetrahedrons (Fig. 1b) [12]. La-
polyhedrons have two common edges with GeO4- and
BO4-tetrahedrons; and common edges in 9-hedrons are
the shortest ones.
Under thermal treatment at low-temperature (T ~
650…680 °C), the amorphous borogermanate glass
transforms into two different chemical phases with
developed interface. However, the homogeneous bulk
crystallization do not proceed [13], because none of
them contains a nuclear of the stillwellite phase.
Homogeneous crystallization (or the so-called
“crystallization without catalyst”) in such glass systems,
according to Ya. Fedorovsky’s studies [14], realizes by
diffusion processes of the glass crystal structure
reconstruction with oxygen-cationic tetrahedral and
polyhedral functional groups presented in solid glass
composition. These processes are of considerable
activation energy, thus requiring certain kinetics
stimulus. In general, the thermodynamic conditions for
the realization of homogeneous nucleation in bulk are
presented. However, much higher temperature is
required than that of growth and development of the
LBG phase on the defects or/and heterogeneous surface
presented in the bulk glass after synthesis (the so-called
heterogeneous nucleation). According to the XRD
analysis data (Fig. 2a) heterogeneous selection of
1 Composition LnBGeO5 (Ln – La, Pr) is characterized by
polymorphism
Semiconductor Physics, Quantum Electronics & Optoelectronics, 2016. V. 19, N 3. P. 267-272.
doi: 10.15407/spqeo19.03.267
© 2016, V. Lashkaryov Institute of Semiconductor Physics, National Academy of Sciences of Ukraine
269
Fig. 1. Fragment of the LaBGeO5 stillwellite structure. Translationally identical columns and B-chains of tetrahedrons (a). Motive
of ВО4- and GeO4-tetrahedrons in the projection on a plane, which is normal to the helical axis of the third order (b).
crystallites from the amorphous matrix into crystalline
phase in the LBG-system takes already place at ca.
650…700 °C. Therefore, at the process stage when
thermodynamic conditions correspond to the realization
of the bulk nucleation process, the major glass structures
are already crystalline and consisted of anisotropic
crystallites of large size. Thus, formation of the well-
distributed nanodispersed crystalline phase in a bulk of
the LBG-glass under normal conditions is virtually
impossible.
Differential thermal analysis showed significant
differences in nature of relaxation processes in the
reference and PMF treated at room temperature samples
(Fig. 3).
There are two individual exothermic peaks (Fig. 3).
Wide low-temperature peak is associated to the
processes of amorphous matrix structural relaxation into
the crystalline state transformation. The high-
temperature peak is associated to the crystallization.
Fig. 2. XPD data of the LaBGeO5 glass crystallization, where:
1 – 750 °C, 2 – 700 °C, 3 – 600 °C. Pure crystalline phase
reflexes appear at T ≥ 700 °C.
The glass verification temperature (Tg) of 670 °C
is situated between two exothermic peaks. In case in
Fig. 1b, a high-temperature peak is more narrow than
in Fig. 2a, which testifies to the less term of
crystallization of PMF-standards, as compared to the
reference. Temperature of the PMF glass crystallization
(close to 805 °C) is of 35 °C above crystallization
temperature for the reference sample (of 770 °C).
Therefore, crystallization of the PMF glass starts later,
but runs faster than for the reference sample.
Temperatures of the maximum of exothermal events
for the reference and the PMF treated samples are,
respectively, of 870 and 880 °C.
Fig. 3. DTA data for (a) reference and (b) PMF treated (f =
1 Hz) LaBGeO5 glass systems (samples weight is of 0.51 g and
0.5 g, respectively; the dynamic mode; air atmosphere; heating
rate 5 deg. × min–1).
The main difference is observed for the relaxation
peaks. It is narrower for the PMF sample with a
Semiconductor Physics, Quantum Electronics & Optoelectronics, 2016. V. 19, N 3. P. 267-272.
doi: 10.15407/spqeo19.03.267
© 2016, V. Lashkaryov Institute of Semiconductor Physics, National Academy of Sciences of Ukraine
270
maximum shifted to a low temperature range down to
100 °C. This fact indicates that relaxation process in the
PMF sample is accomplished earlier than that in the
reference one. Therefore, PMF irradiation accelerates the
preparatory stage of an amorphous matrix for
crystallization.
The dilatometric data indicates a significant
influence of PMF pre-treatment on glass transformation
at all the subsequent stages of structural evolution. It has
to be noted that when the relaxation processes are rapid,
the crystallization of the irradiated materials starts later
than those in the reference sample.
X-ray analysis reveals that the content of LBG-
phase in the PMF treated samples is superior of 30% as
compared to the reference one.
Slight changes in the samples transparency is
identified after their X-ray irradiation. ESR profiles
present a single line for both the reference and PMF
treated samples (Fig. 4). The peak intensity, at the same
line width of 48.5 Gauss and the g-factor values of
g⊥ = [1.9907±0.0003] and g║ = [2.020±0.0003] and
taking into account the samples weight, for the PMF
treated sample is higher than that for the reference one.
These parameters, considering the error of
measurements, are typical for E'-centers, which represent
broken interatomic bonds [15]. The high peak intensity
of the PMF sample (Fig. 4) indicates diffusion of oxygen
within Ge-octahedron, and redistribution of oxygen
atoms resulted in reduction of the corresponding
concentration gradients. Therefore, the PMF pre-
treatment (T ≈ 27 °C, f = 1 Hz) followed by annealing at
500 °C leads to glass homogenization at the atomic
level. Further temperature increase (up to 650…680 °C)
reveals the difference between reference and PMF-
treated samples already at a microscopic level.
Fig. 4. ESR spectra of the (1) reference (172 mg) and (2) PMF-
treated (196 mg) samples annealed at 500 °C for 2 h. Etalon is
Cr3 + in Al2O3.
Optical microscopy reveals a better dispersion and
homogeneous distribution of the nuclear in a bulk of the
irradiated PMF samples as compared to the reference
one (Fig. 5a). Therefore, PMF pre-treatment decreases
the crystallite size and increases the tightness and
density of their distribution in the glass surface layers.
Further temperature increase (> 700 °C) leads to an
increase in the grain size in content of the crystalline
phase and appearance of texture in the directions (200)
and (110) [16].
4. Formation of nanostructured state
in the LBG-glass
Accomplished investigations prove that the effectiveness
of PMF treatment increases with additional thermal
treatment along with annealing at temperature of phase
separation of the glass matrix, i.e., at 650…680 °C.
Formation of the bulk nanodimensional crystalline
structures in glass with crystallite size close to 30 nm
was detected by TEM analysis for the PMF-treated
sample, while the crystallite size of the reference sample
still being in a microscopic range. Pre-treatment
conditions was as follows: PMF treatment (f = 1 Hz) at
27 °C for 1 h, followed by annealing at 600 °C, 2 h
(without PMF); then by PMF treatment (f = 1 Hz) using
step-by-step heating from 650 to 680 °C for 6 h (i.e.,
with the step of 5 °C) and annealing at 705 °C, 2 h
(Fig. 5b). Thus, one can conclude that effects of PMF
pre-treatment both at the stage of phase separation and at
the beginning of glass crystallization are responsible for
the changes in crystallization process character from
heterogeneous (surface) towards the homogeneous one
(bulk).
Fig. 5. Polarization optical microscopy (×400) of the
crystalline phase dispersion at the glass surface. Crystallization
at 705 °C, 2 h: (a) PMF pre-treated sample by using the
frequency close to 1 Hz; and (b) reference sample.
Semiconductor Physics, Quantum Electronics & Optoelectronics, 2016. V. 19, N 3. P. 267-272.
doi: 10.15407/spqeo19.03.267
© 2016, V. Lashkaryov Institute of Semiconductor Physics, National Academy of Sciences of Ukraine
271
Fig. 6. TEM data. Crystal structure of glass formed by the following annealing conditions: a) T = 600 °C, 2 h at step-by-step
heating from 650 up to 680 °C, for 6 h with the step of 5 °C and annealing at 705 °C, 2 h; b) PMF treatment (f = 1 Hz) at 27 °C,
1 h, followed by annealing at 600 °C, 2 h; then by PMF treatment (f = 1 Hz) at step-by-step heating from 650 up to 680 °C, 6 h
with the step of 5 °C and annealing at 705 °C, 2 h.
5. Interpretation of results
All the above mentioned findings suggest that PMF
treatment under certain thermodynamic conditions (such
as heat treatment, X-irradiation) leads to a
homogenization of the material structure from subatomic
(Fig. 4) to microscopic levels (Fig. 5) [17]. In terms of
thermodynamics, it means a transition of the solid-phase
disperse system to a state with a lower free energy (in
this case, the lowest free energy corresponds to the
crystalline state) and is in agreement with well-known
PMF effects in condensed matter.
From the point of view that glass is a supercooled
liquid [18, 19], the delay of crystallization (according to
DTA data) via homogenisation of the structural elements
distribution (according to ESR data) and its further
acceleration (according to DTA data) could be a
consequence of an artificial increase of a “supercooling”
level, i.e., an artificial increase of the amorphous glass
matrix resistance to crystallization. The authors suggest
that course of the processes occurring in the LaBGeO5
upon PMF exposure follows abovementioned principles.
According to DTA data (the relaxation exothermic
peak), the magnetic-induced homogenization of the glass
matrix occurs at relatively low (300…500 °C)
temperatures [20]. Taking into account that formation of
the crystalline structure in the LBG-glass occurs due to
association of the oxygen-cationic tetrahedral and
polyhedral functional groups presented in the glass solid
solutions (such as Ge-, B-tetrahedron, and La-
polyhedron) [21-23], the role of PMF treatment becomes
to be evident in shortage of oxygen ions. Namely, PMF
treatment (i) aligns the existing concentration gradients
of the oxygen vacancies by destruction of defective
complexes2); (ii) blocks association of functional groups
2) According to [20-23] weak magnetic field removes the ban on
electronic transitions with spin inversion, which contribute to reducing
with a specific atomic order; and (iii) constrains
formation of nuclei of critical sizes on the surface
defects below crystallization temperature range.
Therefore, PMF treatment increases potential interaction
of the partially ordered glass elements, thus reducing the
efficiency of the processes of heterogeneous nucleation.
At the temperature when a majority of partially
ordered functional elements located in a bulk glass are
getting enough energy to overcome an activation barrier
of nucleation, a rapid transformation of the glass to the
glass-crystalline state occurs. According to the optical
and electron microscopy data, phase differentiation
displays mainly a bulk behavior (Fig. 6). According to
the DTA data, increase of the temperature of activation
of the crystallization process leads to the formation of a
more dispersed nuclei as compared with the reference
sample, which is similar to the case of “supercooled”
solid solution crystallization.
6. Conclusions
It has been shown that PMF pre-treatment can
significantly affect the kinetics of the structure formation
in the LaBGeO5 glass. Namely, under certain conditions
PMF pre-treatment can alter the character of
crystallization from the surface to bulk matter and
increase the degree of homogeneity of the materials at
micro- and submicron scale levels. The proposed
fundamentally new approach is of practical importance
due to its high potential. Namely, physical modification
of the glass with surface crystallization using
electromagnetic irradiation can be used for controlled
synthesis of new bulk nanostructured glass materials
with a unique complex of electrophysical properties for
modern communication technologies and technology of
nonlinear optics.
the chemical bonds in the defect complexes, whereas, structural
alterations occur due to thermal and elastic energy of the crystal lattice.
Semiconductor Physics, Quantum Electronics & Optoelectronics, 2016. V. 19, N 3. P. 267-272.
doi: 10.15407/spqeo19.03.267
© 2016, V. Lashkaryov Institute of Semiconductor Physics, National Academy of Sciences of Ukraine
272
Acknowledgements
Authors express gratitude to Prof. A. Litovchenko from
Institute of Geochemistry, Mineralogy and Ore after
N.P. Semenenko, NAS of Ukraine for their assistance
with the ESR analysis and data interpretation.
This work was supported by the NATO Science for
Peace Program (grant no. SfP-977980).
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