Journal of Rare Earths 40 (2022) 29e33

Contents lists available at ScienceDirect

Journal of Rare Earths

journal homepage: http://www.journals.elsevier.com/journal-of-rare-earths

Effects of europium concentration on luminescent and scintillation

performance of Cs0.2Rb0.8Ca1
xEuxBr3 (0  x  0.08) crystals*
N.V. Rebrova a, *, A.Yu. Grippa a, I.A. Boiaryntseva a, P. Berastegui b, T.E. Gorbacheva a,

d, e, L. Martinazzoli d, e, E. Auffray e,
Yu.N. Datsko a, A.L. Rebrov a, C. Dujardin c, R. Cala
a
V.V. Kononets
a
Institute for Scintillation Materials, National Academy of Sciences of Ukraine, Nauky Avenue 60, 61072, Kharkov, Ukraine
b
Department of Chemistry, Ångstro €m Laboratory, Inorganic Chemistry, Uppsala University, P.O. Box 583, 75121, Uppsala, Sweden
c
Claude Bernard Lyon 1 University, CNRS, Institute of Light and Matter, UMR 5306, F-69100 Villeurbanne, France
d
The University of Milano-Bicocca, Piazza dell'Ateneo Nuovo, 1 - 20126, Milano, Italy
e
CERN, EP Department, P.O. Box 1211, Geneva 23, Switzerland

a r t i c l e i n f o a b s t r a c t

Article history: A series of Cs0.2Rb0.8Ca1exEuxBr3 (0  x  0.08) crystals doped with different concentrations of Eu2þ were
Received 22 July 2020 grown using the Bridgman-Stockbarger method. The work describes the influence of Eu2þ concentration
Received in revised form on the luminescent and kinetic properties of Cs0.2Rb0.8Ca1exEuxBr3 crystals, as well as on their scintil-
11 August 2020
lation performance. The maximum in the radioluminescence spectra of these crystals shifts from 439 to
Accepted 24 August 2020
Available online 28 August 2020
446 nm with increasing europium concentration. The scintillation decay times of Cs0.2Rb0.8Ca1exEuxBr3
lengthen with the Eu2þ content. The best light output of 33600 photons/MeV is obtained for
Cs0.2Rb0.8Ca0.93Eu0.07Br3, and the best energy resolution of 6.9% is found for Cs0.2Rb0.8Ca0.94Eu0.06Br3.
Keywords:
Inorganic material
© 2020 Chinese Society of Rare Earths. Published by Elsevier B.V. All rights reserved.
Crystal growth
Luminescence
Rare-earth doped scintillator
X-ray and gamma-ray spectroscopies

1. Introduction
Recently, much attention has been paid to inorganic ternary
halides ABX3 (A ¼ K, Rb, Cs; B ¼ Ca, Sr; X ¼ Cl, Br, I) doped with
Eu2þ, since they are considered as possible efficient scintillators for
X-ray and gamma-ray spectroscopy.1e10 The ternary halides are
relatively cheap and, compared with alkaline-earth halide scintil-
lators BX2, they can be much less sensitive to atmospheric mois-
ture1,11,12 and easily grown in large sizes.13e16
One of the ways to enhance the properties of scintillation ma-
terials is the partial substitution of perfectly isomorphic ions in
them. Theoretical calculations as well as experimental results
reveal that solid solutions have better scintillation performance as
compared with parent compounds.17,18 The properties of ternary
halides ABX3 can be modified by partial substitution of cations A
*
Foundation item: Project carried out in the frame of Crystal Clear Collabora-
tion and supported by the National Academy of Sciences of Ukraine (0119U100764).
* Corresponding author.
E-mail address: nadinr1985@mail.ru (N.V. Rebrova).
and B, as well as anion X. Over the past decade, a number of works
have been aimed at modifying the scintillation properties of
ABX3:Eu2þ crystals via searching for the optimal combination of
cations and/or anions. According to the literature19, the partial
substitution of Cl
by Br
resulted in improvement of light yield for
CsCa0.95Eu0.05Cl3exBrx crystals over CsCaCl3:Eu2þ and CsCaBr3:Eu2þ.
A detailed investigation of mixed CsCaI3exBrx:Eu2þ crystals showed
that CsCaI2.2Br0.8:Eu2þ exhibits better scintillation performance and
optical quality than CsCaI3:Eu2þ crystals.20,7 In the further work the
same authors found that CsSrBrI2:Eu2þ, CsCaBrI2:Eu2þ and
CsSrClBr2:Eu2þ also show improved scintillation characteristics
compared with the parent ternary halides.21 It should also be noted
that an excellent scintillator KCa0.8Sr0.2I3:Eu2þ was obtained by
partial replacement of Ca2þ with Sr2þ in KCaI3:Eu2þ.22,23 In a pre-
vious work,24 a significant decrease in hygroscopicity without loss
of scintillation performance was achieved by partially substituting
Sr2þ for Ba2þ in CsSrI3:Eu2þ crystals.
We recently reported a series of Cs1exRbxCa0.95Eu0.05Br3 solid
solutions in which the effect of CseRb substitution on functional
properties was studied.25 Compared with CsCa0.95Eu0.05Br3 and

https://doi.org/10.1016/j.jre.2020.08.012
1002-0721/© 2020 Chinese Society of Rare Earths. Published by Elsevier B.V. All rights reserved.
N.V. Rebrova, A.Yu. Grippa, I.A. Boiaryntseva, et al.
RbCa0.95Eu0.05Br3, the light yield of solid solutions
Cs1exRbxCa0.95Eu0.05Br3 is improved. The best energy resolution of
6.4% was demonstrated by Cs0.2Rb0.8Ca0.95Eu0.05Br3.25 The amount
of Eu2þ doped into the crystal lattice of Cs0.2Rb0.8Ca1exEuxBr3 can
also affect its luminescent and scintillation properties. In this work
we focused on the effect of the Eu2þ concentration on the spectral-
luminescent and luminescence-kinetic properties of
Cs0.2Rb0.8Ca1exEuxBr3 crystals, as well as on their scintillation
performance.
2. Experimental
2.1. Synthesis and crystal growth
The single crystals of Cs0.2Rb0.8Ca1exEuxBr3 (x ¼ 0, 0.005, 0.01,
0.03, 0.05, 0.06, 0.07, 0.08) were prepared from mixtures of the
required compositions of individual components, CsBr, RbBr, CaBr2
and EuBr2. The bromides were synthesized preliminarily from the
powders of Cs2CO3 (99.9%), Rb2CO3 (99.9%), CaCO3 (99.999%) and
Eu2O3 (99.99%), respectively. The synthesis of CaBr2 and EuBr2 is
described in Ref. 26 and the synthesis of CsCl and RbCl is described
in Ref. 25.
The growth procedure using the vertical Bridgman-Stockbarger
method was as follows. The mixtures of the starting materials were
carefully ground in a mortar and loaded into F12 mm  500 mm
quartz ampoules with conical tips. Before growth, the charged
ampoule was pre-heated at 400  C for 5 h under continuous
evacuation to remove the residual water from the charge and then
sealed under vacuum 1.2 Pa. The sealed growth ampoule was
placed into the furnace, and the temperature was slowly raised to
800  C. To achieve good mixing of components, crystal growth was
started after maintaining this temperature for 24 h. The tempera-
ture gradient in the furnace at the growth interface was maintained
at 8  C/cm. The ampoule translation rate through the furnace was
about 3 mm/h. After solidifying the whole melt in the ampoule, the
furnace was cooled down to room temperature at a rate of 10  C/h.
The grown crystals were transparent, some had cracking, but no
visible inclusions were observed (see Fig. 1(a)). The grown boules
were cut to F12 mm  2 mm cylinders (Fig. 1(b)). The slabs were
polished using diamond lapping powders with different grain sizes
(7e40 mm), wrapped by three layers of preliminarily dried Tetratex
tape and housed into aluminum cases to evaluate the luminescent
and scintillation properties.
Fig. 1. (a) Photograph of the Cs0.2Rb0.8Ca0.97Eu0.03Br3 crystal grown by the vertical
Bridgman-Stockbarger method; (b) Polished slabs with sickness of 2 mm are shown in
increasing order of Eu2þ concentration from left to right: 0.5 mol%, 1 mol%, 3 mol%,
5 mol%, 6 mol%, 7 mol%, 8 mol% of Eu2þ.
30
Journal of Rare Earths 40 (2022) 29e33
2.2. Characterization and measurements
Thermal analysis (TG/DTA) for Cs0.2Rb0.8CaBr3 was carried out
on ~40 mg of the sample using a Netzsch STA 409 PC at a heating
rate of 10  C/min under an Ar(g) flow of 70 mL/min up to 850  C.
The instrumental background was corrected by heating an empty
crucible as a blank run.
Measurements of photoluminescence parameters were carried
out in reflectance mode using a combined fluorescent lifetime and
steady-state spectrometer FLS 920 (Edinburgh Instruments)
equipped with a Xe 450 W lamp for steady-state measurements
and hydrogen filled nF 900 ns flashlamp for time correlated single
photon counting measurements. Photoluminescence excitation
(PLE) spectra were corrected for the incident photon flux. Photo-
luminescence emission (PL) spectra were corrected for the spectral
sensitivity of the detection system.
Scintillation decay time profiles of Cs0.2Rb0.8Ca1exEuxBr3
(0.005  x  0.08) were measured on crystals housed in aluminum
casings. Packed samples were placed on the photocathode of
Hamamatsu R6231 PMT using Visilox V-788 as an optical coupling.
Data were obtained using 662 keV gamma radiation from a 137Cs
radioactive source. Signal from photomultiplier tube was fed to the
input of a Rigol DS6064 oscilloscope. Decay profiles were calculated
by averaging of several hundred recorded pulses with amplitudes
roughly corresponding to the full absorption peak.
Room temperature radioluminescence measurements were ob-
tained using a Philips X-ray tube operated at 30 kV. The emitted light
was collected with an optical fiber and recorded by an Andor Newton
EMCCD coupled to an Andor Shamrock 500i monochromator.
The scintillation light outputs were measured under 137Cs
gamma-ray source (661.7 keV). The set-up consisted of a
temperature-controlled black box containing a Hamamatsu R2059
PMT connected to a DT5720A CAEN digitizer performing charge
integration. The PMT bias voltage was 2500 V. The test bench
calibration was based on the measurement of the signal produced
by a single photoelectron escaping the photocathode as in the
literature.27 It employed an integration gate of 16 ms (the largest
allowed by the digitizer) for all the samples, chosen as to
comfortably integrate all the charge produced by the light pulse.
Glycerine was used as optical coupling. The 137Cs source was placed
at a sufficient distance to avoid pile-up. Average quantum efficiency
was calculated using the radioluminescence spectra and the
quantum efficiency of the photodetector. The uncertainty of the
measurement was estimated to be 5%.
To determine the europium concentration in the samples, we
used complexometric titration with a standard EDTA solution and
xylenol orange as an indicator.28e30 The experimentally obtained
content of Eu2þ in the samples using complexometric titration is
close to the nominal one from the chemical weight formula.
3. Results and discussion
3.1. TG/DTA measurements
The TG/DTA curves of Cs0.2Rb0.8CaBr3 are shown in Fig. 2.
Thermogravimetry curve shows a weight loss below 200  C of
1.5%e4% that can be attributed to a loss of adsorbed moisture
during the loading of the sample. A sample that was preheated to
700  C showed negligible weight loss but the same melting point as
a sample exposed to air during the loading in the crucible. A second
weight loss is observed after the onset of the melting temperature
as the sample decomposes. The observed melting temperature of
767  C is between those reported for RbCaBr3 (739  C) and CsCaBr3
(831  C).31
N.V. Rebrova, A.Yu. Grippa, I.A. Boiaryntseva, et al. Journal of Rare Earths 40 (2022) 29e33

Fig. 2. Thermogravimetric analysis (upper trace) and differential thermal analysis

(lower trace) curves of Cs0.2Rb0.8CaBr3.

3.2. Photoluminescence properties

PLE and PL spectra of Cs0.2Rb0.8Ca1exEuxBr3 crystals with different

Eu2þ concentrations are given in Fig. 3 (excitation spectra were
recorded for the long-wavelength side (460 nm) of the emission
spectra). For the sample with trace amounts of Eu2þ, the excitation
spectrum represents two sets of superimposed bands in the
230e280 and 310e410 nm regions. The observed bands are associ-
ated with 4f7/4f65d1 absorption transitions of Eu2þ ions.32,33 For
the samples with a higher Eu2þ content, separate bands are not
distinguishable. This situation is typical for crystals with high dopant
concentrations due to the absorption saturation effect.
Upon excitation with 340 nm light, all the studied samples
demonstrate emission in the blue spectral region arising from the
4f65d1/4f7 radiative transitions of Eu2þ. As can be seen in Fig. 3, an
increase in the europium content in crystals increases the overlap
between the excitation and emission bands. As a result, the position
of the apparent emission maximum gradually shifts toward the
long-wavelength region from 428 to 441 nm due to the well-known Fig. 3. PLE for lem ¼ 460 nm (curves 1, 2, 3) and PL for lex ¼ 340 nm (curves 1', 2', 3')
spectra of Cs0.2Rb0.8Ca1exEuxBr3 crystals at 300 K.
self-absorption effect.34,35
PL decay profiles of Cs0.2Rb0.8Ca1exEuxBr3 crystals measured in
the reflectance mode (from the front surface of the sample) are
shown in Fig. 4. The decay curve of the sample with the smallest
Eu2þ concentration is well fitted by a single-exponential function
with a time constant of about 850 ± 50 ns. At higher Eu2þ concen-
trations, the luminescence decay does not follow the single-
exponential decay law, and the apparent lifetimes are much
longer. The estimated time constants obtained as a result of the fit
using the two-exponential function are approximately 1.1 ± 0.1 ms
and 2e3 ms. The contribution of the first decay component decreases
with increasing europium concentration, while in the case of the
second component we observe the opposite behavior. The observed
lengthening of the apparent decay time with increasing dopant is
common for crystals exhibiting self-absorption due to multiple cy-
cles of light re-absorption and re-emission processes.34e36 It should
be noted that in the case of strong self-absorption, the luminescence
lifetimes recovered by multi-exponential fitting are much longer
than intrinsic ones, and they can only be estimated.
Fig. 4. PL decay profiles for lex ¼ 340 nm, lem ¼ 430 nm of Cs0.2Rb0.8Ca1exEuxBr3
crystals at 300 K.

3.3. Scintillation characterization

Scintillation decay profiles of the studied crystals collected in
transmittance mode are presented in Fig. 5. In order to reduce size-
dependent effects that can substantially affect the test results, all
samples had the same dimension of F12 mm  2 mm. As in the case
of photoexcitation, with an increase of the Eu2þ concentration in
Cs0.2Rb0.8Ca1exEuxBr3, a significant lengthening of scintillation
decay times occurs. The inset shows the concentration dependence
of the time constants extracted from the single-exponential fitting
of the scintillation decay profiles.
Radioluminescence spectra of the samples measured under X-
ray excitation in the reflection mode show a typical Eu2þ ions
emission, which is associated with 4f6/5d14f7 radiative transitions

31
N.V. Rebrova, A.Yu. Grippa, I.A. Boiaryntseva, et al. Journal of Rare Earths 40 (2022) 29e33

Fig. 7. Light output photopeaks for the Cs0.2Rb0.8Ca1exEuxBr3 (x ¼ 0.06, 0.07 and 0.08)
samples (137Cs radiation source).

Fig. 5. Scintillation decay profiles of Cs0.2Rb0.8Ca1exEuxBr3 crystals at 300 K (137Cs

radiation source). Inset: scintillation decay constants vs. Eu2þ concentration.

Fig. 8. Concentration dependence of light yield in Cs0.2Rb0.8Ca1exEuxBr3 crystals at

300 K (137Cs radiation source).
Fig. 6. Radioluminescence spectra of Cs0.2Rb0.8Ca1exEuxBr3 crystals under X-ray exci-
tation at 300 K. Inset: integrated X-ray emission intensity vs. Eu2þ concentration.

(Fig. 6). The emission intensity grows linearly with increasing Eu2þ
concentration. No signs of concentration quenching of radio-
luminescence were observed in the studied concentration range.
Light output photopeaks for Cs0.2Rb0.8Ca1exEuxBr3 (x ¼ 0.06,
0.07 and 0.08) crystals are given in Fig. 7. The light output depen-
dence on activator concentration of the samples is plotted in Fig. 8.
Unlike radioluminescence, the light output reaches a maximum of
33600 photons/MeV at Eu2þ concentration of about 0.07 and starts
to decrease at higher europium content. Since the results obtained
for radioluminescence yield do not reveal any signs of concentra-
tion quenching, it can be assumed that the observed decrease of
scintillation light output in Cs0.2Rb0.8Ca1exEuxBr3 at a dopant level
>0.07 is caused by the radiation trapping in the sample volume. In
the case of radioluminescence, the light trapping effect is negli-
gible, since the emission is registered from a relatively thin near-
surface layer excited by X-rays. The scintillation characteristics for
Cs0.2Rb0.8Ca1exEuxBr3 crystals are summarized in Table 1. The best
energy resolution of 6.9% ± 0.5% was found for
Cs0.2Rb0.8Ca0.94Eu0.06Br3.
4. Conclusions
The Cs0.2Rb0.8Ca1exEuxBr3 crystals were grown using the vertical
Bridgman-Stockbarger method. The luminescent and scintillation

Table 1
Scintillation properties of Cs0.2Rb0.8Ca1exEuxBr3 crystals (137Cs radiation source).

Nominal Concentration X-ray excited Decay Light output (photons/MeV) Energy resolution
concentration of Eu2þ determined luminescence time (ms)
of Eu2þ by titration max (nm)

0.005 0.0052 ± 0.0005 439 2.16 9500 ± 400 12.9% ± 0.6%

0.01 0.0091 ± 0.0008 441 2.59 12100 ± 500 21.1% ± 0.6%
0.03 0.0283 ± 0.0006 443 3.1 27000 ± 1000 26.4% ± 1.3%
0.05 0.0539 ± 0.0004 444 3.5 28100 ± 1100 10.9% ± 0.5%
0.06 0.0597 ± 0.0005 443 3.69 30600 ± 1200 6.9% ± 0.5%
0.07 0.0680 ± 0.0007 445 3.74 33600 ± 1300 8.9% ± 0.5%
0.08 0.0811 ± 0.0004 446 4.34 30000 ± 1200 7.7% ± 0.2%

32
N.V. Rebrova, A.Yu. Grippa, I.A. Boiaryntseva, et al. Journal of Rare Earths 40 (2022) 29e33

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