Article
Cite This: Cryst. Growth Des. 2018, 18, 7435−7440
pubs.acs.org/crystal
Development of a Synthesis Technique and Characterization of
High-Quality Iron Borate FeBO3 Single Crystals for Applications in
Synchrotron Technologies of a New Generation
Sergey Yagupov,† Mark Strugatsky,*,† Kira Seleznyova,† Yuliya Mogilenec,† Nikita Snegirev,†
Nikita V. Marchenkov,‡,§ Anton G. Kulikov,‡,§ Yan A. Eliovich,‡,§ Kirill V. Frolov,‡ Yulia L. Ogarkova,‡
and Igor S. Lyubutin‡
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†
Physics and Technology Institute, V.I. Vernadsky Crimean Federal University, 295007 Simferopol, Russia
Shubnikov Institute of Crystallography of FSRC “Crystallography and Photonics” RAS, 119333 Moscow, Russia
§
National Research Center “Kurchatov Institute”, 123098, pl. Akademika Kurchatova, 1, Moscow, Russia
‡
ABSTRACT: A flux growth technique for synthesizing FeBO3 single crystals of high structural perfection was developed. The
high structural quality of the synthesized FeBO3 crystals was confirmed by means of double-crystal X-ray diffraction analysis
both in Laue and Bragg geometries. The diffraction rocking curves taken locally and integrally over the surface are in excellent
agreement with the calculated curves. Some macrodefects were revealed by X-ray topography in the crystal volume. However,
the local defects do not prevent the use of defect-free regions of the crystal for synchrotron Mössbauer experiments.
1. INTRODUCTION
Traditional Mössbauer spectroscopy, e.g., on 57Fe nuclei, is a
widely used and effective experimental method for studying
structural, electronic, and magnetic properties of various
materials.1 However, the standard procedure is poorly suited
for studying small objects (less than 100 μm) and for experiments under extreme conditions, such as strong magnetic fields,
high temperatures, and also in high-pressure chambers with
diamond anvils.2,3 The traditional method of Mössbauer spectroscopy is based on the use of radioactive sources. However, a
major drawback of this method is the ineffective use of the
radioactive radiation from the Mössbauer source during the
experiments. The Mössbauer radiation is uniformly distributed
over the sphere (in 4π), and only a small part of it falls on the
sample under study. Thus, durable measurements are required
in order to obtain necessary statistics that affects the quality of the
results. In this situation, the possibility of using high-intensity
focused synchrotron radiation in the traditional Mössbauer
scheme instead of the standard nuclear gamma-ray source seems
to be the most effective and optimal one. However, first and
foremost, it is required to distinguish from the “white” synchrotron radiation the interval of radiation with energy corresponding
© 2018 American Chemical Society
to Mössbauer resonance. For this purpose, at the initial stage, a
system of standard monochromators based on silicon crystals is
used.4 However, this system does not provide sufficient tuning
accuracy to the resonant frequency. In order to solve this
problem, recently it has been proposed to use the effect of
nuclear diffraction of Mössbauer radiation in the FeBO3 crystal
on the final stages of monochromatization.5 A special tuning
leads to the contribution in the diffraction process of only
Mössbauer 57Fe nuclei that provide an ideal monochromatization of the diffracted radiation.6−9
This approach has been described in a series of theoretical and
experimental studies.10−13 It was proposed to use iron borate
crystals 57FeBO3 in order to obtain X-ray radiation with characteristics corresponding to the 57Fe resonance absorption line.
FeBO3 has the rhombohedral calcite structure, space group
R3̅c.14 For this crystal all reflections (NNN) ((111), (222),
(333), etc.) are forbidden for electron diffraction, but are
allowed for nuclear diffraction. Such an experimental technique
Received: July 26, 2018
Revised: October 13, 2018
Published: October 23, 2018
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Figure 1. Temperature mode of crystallization used in synthesizing FeBO3 crystals of high structural perfection.
is called “synchrotron Mössbauer spectroscopy” (SMS) and has
been tested and implemented in European Synchrotron Radiation Facility at beamline ID18 (Grenoble, France)6 and also in
SPring-8 (Tsukuba, Japan).15
It was established that X-ray diffraction conditions impose
strict requirements on the high quality of such crystals. In addition, in order to provide the symmetry for the necessary reflections, the crystals must have a shape of a basal plate with the
plane parallel to the plane of reflection (NNN). Moreover, the
required crystals should be enriched up to 95% with the 57Fe
isotope.
Meanwhile, at present, the deficit of FeBO3 single crystals of
high structural perfection that, as mentioned above, are a key
element of the SMS, imposes significant limitations on the
further development of this technique. Iron borate crystal
synthesis can be implemented by (i) vapor, see, e.g.,16,17 and
(ii) flux, see, e.g.,18,19 growth. Using technique (i), bulk single
crystals of iron borate with large nonbasal faces can be obtained.
Meanwhile, technique (ii) allows obtaining single crystals with
the shape of basal plates. Such crystals are of high structural
perfection19 and possess large basal faces, which is difficult to
obtain by technique (i). Thus, for the purposes of the present
work the flux growth technique has proved to be most appropriate. However, a standard route of crystal synthesis has to be
modified in order to avoid mechanical stresses and destruction
of large crystals.
The aim of the present work is to develop a technique for
synthesis FeBO3 single crystals of high structural perfection
suitable for applications in synchrotron technologies and to
determine the degree of their structural perfection by X-ray
diffraction (XRD) analysis.
Iron borate crystals are usually synthesized in the (i) Fe2O3−
B2O3−PbO−PbF2, see, e.g.,18−22 and (ii) Fe2O3−B2O3−Bi2O3,
see, e.g.,23,24 systems. Meanwhile, the latter system destructively
acts on the platinum crucible. Moreover, FeBO3 crystals synthesized using the (ii) system usually possess Bi as an impurity.
Thus, the crystallizations were carried out in the (i) system. The
crystal-forming reagents are Fe2O3 and B2O3; PbO, PbF2, and
B2O3 serve as solvents. Note that B2O3 is both crystal-forming
reagent and solvent. A typical composition of the reagents used
for successful synthesis of FeBO3 crystals in wt % is as follows:
Fe2O3 (5.73), B2O3 (51.23), PbO (29.31), and PbF2 (13.73).
After a charge composition was determined, all reagents were
dehydrated separately in a drying chamber at 150 °C during
24 h. Next, the reagents were weighed with a high-precision
balance and mixed with a laboratory-developed device.
For obtaining a homogeneous solution melt, small portions,
about 5 g, of the charge were successively adjoined to a platinum
crucible (with a volume of 90 cm3) and each time kept for
20 min in a muffle furnace at 870 °C. The weight of the melt
solution was 137.1 g.
The crucible with the prepared solution melt was covered
with platinum foil perforated with small holes and another similar crucible (crucible-lid with a volume of 75 cm3) and installed
in the crystallization furnace with uniform temperature distribution. The junction between the crucibles was neatly rolled.
Figure 1 shows a typical temperature regime used in synthesizing FeBO3 crystals. It includes the following steps:
(i) heating of the furnace from the room temperature;
(ii−iii) a few cycles of homogenization of the solution melt with
subsequent sharp temperature dropping in order to
improve the homogeneity of the solution-melt (in particular, without the application of this technique, solid
deposits were found on the bottom of the crucible) and
to avoid the emergence of spurious phases, e.g., Fe3BO6;
(iv) cooling of the furnace with a speed of 0.5 °C/h (during
this step crystal growth occurs);
(v) furnace overturn (during this step the solution melt was
drained into a crucible-lid);
(vi) cooling the furnace.
After the last step, a crucible was removed from the furnace
and uncovered. The solidified solution melt and several large
single crystals of iron borate have turned out to be, respectively,
in the crucible-lid and on the foil perforated with small holes.
We emphasize the importance of the separation of the liquid
solution melt from the synthesized crystals at high temperatures.
2. SYNTHESIS OF FeBO3 SINGLE CRYSTALS OF A HIGH
STRUCTURAL PERFECTION BY THE FLUX GROWTH
TECHNIQUE
The synthesis of FeBO3 single crystals of a high structural
perfection by flux growth technique includes the following steps:
(i) determining suitable charge compositions and temperature
modes; (ii) preparing the charge; (iii) obtaining a homogeneous
solution melt in a platinum crucible; (iv) slow cooling of the
solution melt according to a predetermined temperature mode;
(v) separation of synthesized crystals from the liquid solvent by
draining the latter at high temperature. All the parameters of
crystallization are interdependent. Therefore, achievement of
the best results requires optimization of each technological step.
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Figure 2. (a−c) Examples of the synthesized FeBO3 single crystals.
Figure 3. Schematic diagram of the experimental setup (TXS) for obtaining double-crystal DRCs and topograms.
their bigger size and, thus, more convenience of working with
them.
XRD studies were carried out with a triple-axis X-ray spectrometer (TXS), the principal scheme of which is shown in
Figure 3. The sample and the detector were mounted on a tripleaxis goniometer with a set of lateral movements for precise
alignment of the sample. An X-ray tube with a Mo anode with a
wavelength of characteristic radiation Kα1 λ = 0.7093 Å served as
a radiation source. The monochromatization block includes the
slits for preliminarily collimation installed before the crystalmonochromator, and the silicon monochromator itself, see
Figure 3. In order to detect the scattered X-ray radiation, a
scintillation detector was used to measure the double-crystal
DRCs. A two-coordinate Bruker detector with the CCD matrix
resolution of 1024 × 1024 pixels and a pixel size of 100 μm was
used in order to record the topograms.
The experiments have been carried out in Laue (for X-ray
transmission, reflection (3 3̅ 0) with a diffraction angle of 15.42°
and extinction length Lext = 85.8 μm) and Bragg (for X-ray
reflection, reflection (0 0 12) with a diffraction angle of 17.09°
and Lext = 8.7 μm) geometries.
A DRC is a dependence of the intensity of the monochromatic
X-ray radiation scattered by the crystal on the diffraction angle,
which is varied near the Bragg angle. The shape and half-width of
the curve allow judging the presence of a defective structure of
the crystal lattice in the volume of interaction with the X-ray
beam. In order to measure the double-crystal DRCs we used a
symmetric single Si crystal tuned to the (220) reflex. For
obtaining integral DRCs the sample was illuminated over the
whole surface by a wide monochromatic X-ray beam; for DRCs
with a high spatial locality collimating slits were installed in
addition after the monochromator to restrict the beam projection on the sample up to several square millimeters.
The topogram provides a visual representation of the distribution of the defects basing on the changing of the intensity of
If such a separation does not occur, the crystals are exposed to
thermal deformations of solidified solution melt that lead to the
destruction of large crystals and the occurrence of mechanical
stresses in them.
Total weight of the synthesized crystals was 5.2 g. The synthesized crystals have the shape of odd crystal pieces and correct
(hexagonal) plates with the dimensions up to 15 mm and 5 mm
in the basal plane, respectively, and ca. 180 μm in the perpendicular direction. Examples of the synthesized samples are
shown in Figure 2. It should be noted that spurious phases, e.g.,
Fe3BO6, are absent.
Our thorough studies have shown that the optimal composition of the reagents is similar to that used previously, see, e.g.,
refs 18 and 19. However, we significantly improved temperature
mode of crystallization, which led to an increase of the degree of
structural perfection of the synthesized samples. Moreover, we
managed to avoid the appearance of spurious crystalline phases.
For this purpose, we have developed a microprocessor system,
which allows controlling the temperature mode of crystallization
with high accuracy and speed. The mass of the solution-melt and
the volume of the crucible that we used exceed that used by the
authors in the work,18 which makes it possible to obtain more
crystals. It should be noted, that in refs 19 and 20 the procedure
of furnace overturn is absent; meanwhile, it is crucial for
obtaining large crystals of a high structural perfection.
3. CHARACTERIZATION OF THE SYNTHESIZED
SINGLE CRYSTALS
In order to determine the degree of crystalline perfection, the
synthesized crystals were studied by means of double-crystal
XRD analysis. The double-crystal diffraction rocking curves
(DRCs) of iron borate with various degrees of localization of
the crystal illumination by an X-ray beam, as well as X-ray
topograms, were obtained. We have chosen to carry out measurements on odd-shaped crystal pieces, see Figure 2a,b, due to
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Figure 4. Local experimental (a and b) and calculated (c and d) double-crystal DRCs of FeBO3 crystal obtained with a high spatial locality.
diffracted X-ray radiation over the whole area of the crystal.25
Dynamic scanning mode with a simultaneous rotation in angular
range of 150 arcseconds and total time exposure of about 300 s
was used: the integral intensity of the double-crystal DRC
accumulates from each point of the surface.26 This mode shows
the differences in the integral intensity associated with the structure heterogeneity. At the same time, it excludes the contribution of a possible influence caused by the crystal holder since the
integral intensity is not sensitive to the slight bending of the
crystal. The size of the point (without taking divergence into
account) is determined by the resolution (pixel size) of the 2D
detector.
For the X-ray topography method, an asymmetric silicon
monochromator of the slice (440) with an asymmetry coefficient of b = 0.025 was used. Asymmetric cut allows creating a
spatial broadening of the initial beam in the plane of diffraction
that ensures uniform illumination of the whole sample surface
with a monochromatic radiation.
Figure 4a,b shows the local double-crystal DRCs. As one can
see, they have a symmetrical shape and the values of the halfwidth (fwhm) of the DRCs obtained in Laue and Bragg
geometries are 12.4 and 16.3 arcsec, respectively.
Figure 4c,d shows the results of numerical modeling of the
double-crystal DRCs. The calculations were carried out in
accordance with the dynamic theory of diffraction taking into
account the structural factor of this crystal, the instrumental
function of the source ,and the Si monochromator convolution
with allowance for the dispersion effect.27,28 The calculated
curves are in a good accordance with experimental data, which
testifies a high perfection of the obtained FeBO3 crystals.
The reason for the broadening of the curve in the Bragg
geometry in comparison with Laue geometry lies in different
depths of extinction, which in these two cases differs by an order
of magnitude, vide supra. According to calculations for selected
reflections, in the case of diffraction in Bragg geometry the
information is collected from a volume corresponding to a nearsurface layer of about 7 μm in depth due to the small extinction
length. As far as crystal surface itself represents a structural
defect, the DRCs measured in Bragg geometry have larger values
of fwhm It is possible that this broadening is due to the additional defects associated with the reconstruction of the surface of
the crystal.29,30
In order to estimate the homogeneity and crystal quality of the
whole sample volume, the integral double-crystal DRCs were
also measured, see Figure 5. The estimated fwhm values of
the DRCs are about 50 arcsec. Thus, local experimental DRCs
made it possible to establish that a significant part of the crystal
volume has a high structural perfection. Some broadening of
integral DRCs may be due to the existence of some localized
macroscale defects observed on topograms (see below). The
total volume of these defects is relatively small.
The following factors can contribute to the broadening of the
double-crystal DRCs in both Laue and Bragg measurement
schemes:
(i) The effect of X-ray beam dispersion due to the difference
in the diffraction angles of the monochromator and the
sample;
(ii) Possible bending of a thin crystal due to the mechanical
impact that appears from the crystal holder;
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Figure 5. (a, b) Integral experimental double-crystal DRCs of FeBO3 crystal.
Figure 6. X-ray topograms of the FeBO3 crystals: (a) sample on Figure 2a in the Bragg geometry, (b) sample on Figure 2b in the Bragg geometry,
(c) sample on Figure 2b in the Laue geometry.
(iii) The presence of different defects in structure and the
disrupted near-surface layer.
ORCID
The cause (i) can be added to the calculations, and the remaining
two can only be verified experimentally by the topography.
The topograms of two samples, shown in Figure 2a,b, were
measured in the Laue and Bragg geometries, see Figure 6. The
topography reveals the crystal regions with a different integral
intensity. In particular, the clearly visible dark spots indicate the
presence of growth defects and microcracks in the sample
volume. However, these localized defects do not prevent the use
of defect-free regions of the crystal.
Notes
Mark Strugatsky: 0000-0002-9282-5768
The authors declare no competing financial interest.
ACKNOWLEDGMENTS
■
REFERENCES
This work was partially supported by the Russian Foundation for
Basic Research (RFBR) and the Ministry of Education, Science
and Youth of the Republic of Crimea in the framework of
scientific project Grant nos. 16-42-910593 and 17-42-92015
“p_a”, by the RFBR in the framework of scientific project Grant
no. 18-32-00210 “mol_a” (synthesis of experimental samples)
and by the V.I. Vernadsky Crimean Federal University
Development Program for 2015−2024. Support by RFBR
Grant No. 17-02-00766 in part of the Mössbauer spectroscopy
characterization and by the Ministry of Science and Higher
Education within the State assignment FSRC “Crystallography
and Photonics” RAS in part of the X-ray diffraction analysis are
also acknowledged.
4. CONCLUSION
We have succeeded in obtaining high-quality FeBO3 single crystals using the flux growth technique. The latter one was substantially modified in order to avoid the destruction of large crystals
and the occurrence of mechanical stresses in them, and to
eliminate the formation of spurious crystalline phases during the
synthesis. By means of XRD analysis, we confirmed a high degree
of structural perfection of the synthesized FeBO3 crystals. The
double-crystal DRCs taken over the surface are in excellent
agreement with the calculated curves for perfect crystals. In the
crystals studied, some macrodefects revealed by X-ray topography
in the crystal volume may be associated with cracks occurred
during the synthesis. However, these defects will not affect the
efficiency of Mössbauer diffraction initiated by a synchrotron
beam passing in the defect-free regions of the crystal. The
synchrotron Mössbauer experiments on the synthesized samples
are in progress and will be published elsewhere.
■
■
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AUTHOR INFORMATION
Corresponding Author
*Phone: +79787870106. E-mail: strugatskymb@cfuv.ru.
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