Journal of Crystal Growth 490 (2018) 84–88

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Journal of Crystal Growth

journal homepage: www.elsevier.com/locate/crys

Characterization of CuCl quantum dots grown in NaCl single crystals via

optical measurements, X-ray diffraction, and transmission electron
microscopy
Kensuke Miyajima ⇑, Tatsuro Akatsu, Ken Itoh
Department of Applied Physics, Graduate School of Science, Tokyo University of Science, 6-3-1 Niijuku Katsusika-ku, Tokyo 125-8585, Japan

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

Article history: We evaluated the crystal size, shape, and alignment of the lattice planes of CuCl quantum dots (QDs)
Received 6 November 2017 embedded in NaCl single crystals by optical measurements, X-ray diffraction (XRD) patterns, and trans-
Received in revised form 18 February 2018 mission electron microscopy (TEM). We obtained, for the first time, an XRD pattern and TEM images for
Accepted 6 March 2018
CuCl QDs in NaCl crystals. The XRD pattern showed that the lattice planes of the CuCl QDs were parallel to
Available online 7 March 2018
Communicated by R. Fornari
those of the NaCl crystals. In addition, the size of the QDs was estimated from the diffraction width. It was
apparent from the TEM images that almost all CuCl QDs were polygonal, although some cubic QDs were
present. The mean size and size distribution of the QDs were also obtained. The dot size obtained from
Keywords:
B1. Cuprous chloride
optical measurements, XRD, and TEM image were almost consistent. Our new findings can help to reveal
A1. Nanostructures the growth mechanism of semiconductor QDs embedded in a crystallite matrix. In addition, this work
A1. Characterization will play an important role in progressing the study of optical phenomena originating from assembled
A1. X-ray diffraction semiconductor QDs.
A1. Transmission electron microscopy Ó 2018 Elsevier B.V. All rights reserved.
B1. Sodium chloride

1. Introduction
Research on the optical properties of an exciton, an electron–
hole pair coupled through Coulomb’s interactions, confined in a
semiconductor nanoparticle has been performed extensively about
the last three decades [1–3]. In semiconductor nanoparticles,
quantization of the energy levels of the exciton occurs due to the
quantum size effect [4–6]. Such nanoparticles are referred to as
quantum dots (QDs). Fundamental properties regarding to size-
dependent energies and relaxation processes of an exciton or
multi-exciton have been investigated for many types of QDs
[7,8]. A variety of techniques to prepare QDs have been established.
For applications in optoelectronic devices, in general, QDs are
grown on substrates through self-organization via the Stranski-
Krastanov growth mode (S-K mode) [9–13]. The preparation of
QDs in organic solvents [14–17], polymers [18,19] and inorganic
matrices [20–27] have also been performed extensively. In terms
of inorganic matrices, QDs embedded in glass matrices are very
common, being used in commercial colour filters. To date, most
reports are of QDs prepared from II-VI compounds [20,21,23] or
I-VII compounds [20–22,24,25]. Copper halide nanocrystal fabrica-
⇑ Corresponding author.
E-mail address: miyajima@rs.tus.ac.jp (K. Miyajima).
tion e.g. CuCl, CuBr and CuI, within alkali-halide crystals, e.g. NaCl,
KCl or KI, have also been reported [26,27].
In this paper, we report the characteristics of CuCl QDs embed-
ded in NaCl single crystals. CuCl QDs exhibit a quantum size effect
in a weak confinement regime, in which the centre-of-mass motion
of the exciton is quantized. This is because the effective Bohr radius
of the exciton is 0.7 nm, which is smaller than the typical radius of
CuCl QDs. There are many interesting phenomena associated with
an exciton confined in a CuCl QD: exciton superradiance [28,29],
large optical nonlinearlity [30–32], and a narrow homogeneous
width [33–35]. Furthermore, recently, superfluorescence, which
is a cooperative spontaneous emission from multiple excited
two-level systems that are coherently coupled by a radiation field,
has been reported for the high-density ensemble of CuCl QDs
[36,37]. For such a coherent phenomenon or macroscopic dynam-
ics of the ensemble of QDs, a synthetic method is required to pro-
duce a high-density assembly of QDs with narrow size distribution.
Previous reports investigating the optical properties of CuCl
QDs used glasses [20,25,26,29–35], NaCl crystals [27,28,32–37],
and polymethyl methacrylate (PMMA) [38] as a host matrix. The
TEM image of CuCl QDs was shown for a sample of QDs produced
by magnetron RF sputtering in glass [25]. However, as opposed to
optical measurements, there are few reports analyzing the size and
shape of QDs by TEM and X-ray diffraction (XRD). Particularly, TEM
and XRD characterization of CuCl QDs grown in NaCl single crystals

https://doi.org/10.1016/j.jcrysgro.2018.03.010
0022-0248/Ó 2018 Elsevier B.V. All rights reserved.
 K. Miyajima et al. / Journal of Crystal Growth 490 (2018) 84–88
have not been reported. The sizes and shapes of CuCl QDs in NaCl
single crystals have mainly been evaluated by optical measure-
ments. T. Itoh et al. reported the sizes of CuCl QDs by analyzing
small angle X-ray scattering (SAXS) and photoluminescence (PL)
peak energies, where it was suggested that the shapes of the QDs
are spherical [27]. Y. Masumoto et al. calculated the quantized
energy levels of excitons in QDs measured by absorption spectra
and the spectral hole-burning measurement [39]. The obtained
energy levels indicated that the QDs were not spherical but cubic.
Cubically shaped CuCl QDs in NaCl matrices were also reported
using scanning near-field microscopy (SNOM) [40]. In addition,
D. Fröhlich reported that the lattice planes (1 0 0) of CuCl QD were
parallel to the cleaved (1 0 0) surface of a NaCl single crystal using
the selection rule of two-photon absorption of the exciton [41].
When the matrix is an alkali halide crystal, QD shape and the
alignment of its lattice planes should be influenced by its sur-
roundings. As opposite to diffusion-controlled growth in glass
matrices, the growth mechanism of QDs in crystalline matrices
has not been deciphered. The structural characteristics of QDs
affect the obtained optical properties. For example, differences in
the homogeneous width of the exciton are observed for glass
matrices and NaCl single crystals [35]. Since the generation of
superfluorescence requires coherent coupling between the dipole
moments in the QDs, the homogeneous width of QDs is critical.
Study of the size, shapes, and structure of QDs embedded in a sin-
gle crystal is important to elucidate the effect of a surrounding
matrix on the QDs, and for studying the optical phenomena origi-
nating from QD assembly.
In this study, we examined the optical spectra, XRD patterns,
and TEM images of CuCl QDs embedded in NaCl single crystals to
determine the size, shape and alignment of lattice planes of the
QDs. The samples were prepared with a higher concentration of
CuCl compared to a previous report [27] because this current arti-
cle produced materials to study the generation of superfluores-
cence. XRD and TEM images for the CuCl QDs grown in NaCl
crystals are reported for the first time in this paper.
2. Experimental setup
CuCl QDs embedded in NaCl matrices were fabricated by the
transverse Bridgman method, followed by an annealing process.
First, NaCl and CuCl powders were sealed in a quartz ampoule with
Ar gas at a pressure of 1/3 atm. The concentration of CuCl was 10
mol%, which is higher compared to previously reported values [27].
The sealed quartz ampoule was placed in a furnace where the tem-
perature of 820 °C was maintained, which is above the melting
point of both NaCl and CuCl (801 °C and 426 °C, respectively).
The furnace was moved horizontally at a speed of
1.7 cm/day.
Consequently, opaque NaCl crystals with CuCl inclusions were
obtained. Next, we annealed these crystals in Ar at 650 °C for 24
h. As a result, CuCl QD (which are nanometer-sized particles)
assemblies were obtained within NaCl single crystals, which
became transparent. During the annealing process, the concentra-
tion of CuCl decreased due to the evaporation of CuCl from the
NaCl matrix. The X-ray fluorescence measurements showed that
the actual concentration of CuCl was approximately 0.2 mol%. For
further measurements, we prepared three samples: NaCl crystal
with CuCl QD inclusions after annealing, NaCl crystal with CuCl
inclusions before annealing, and NaCl crystal without CuCl inclu-
sions, with the same technique described above.
Optical measurements, that is, absorption and photolumines-
cence (PL) spectroscopy, were performed at 77 K. An ultraviolet
(310-nm wavelength) light emission diode (LED) was used as the
excitation source for PL measurements. The spectra were analyzed
using 50 cm-focal length spectrometer (Acton; SP2500i, 2400
85
grooves/mm) equipped with a charge-coupled device (Roper; PIX-
IS100B). XRD analysis was performed using an apparatus (RIGAKU;
Smartlab) with the Ka line of Cu (k = 1.541 Å). For optical and XRD
measurements, the samples were cleaved as platelets with a thick-
ness of
0.5 mm on the (1 0 0) plane of the NaCl crystal. TEM
devices (NipponDenshi; JEM200EX or Hitachi; H-9500) were used
to observe the CuCl QDs in the NaCl crystal. The NaCl crystals with
the CuCl QD inclusions were crushed and then dispersed in acetone
by sonicating the sample for 15 min. The weight ratio of NaCl crys-
tals to solvent was 3:2.
3. Results and discussion
3.1. PL and absorption spectra
The PL and absorption spectra of CuCl QDs in NaCl crystal at
77 K are shown in Fig. 1. The peak energies of 3.2302 and
3.2268 eV were observed at 77 K for the absorption and PL spectra,
respectively. The lower values of the PL peak energy compared to
absorption ones can be attributed to reabsorption or bound states
of the excitons. We evaluated the average effective dot radius using
the absorption peak energy. When we consider the exciton energy
confined in a spherical dot for the weak confinement regime, the
energy shift of the exciton, DE, compared to that in bulk is
expressed by
h2 p2
DE ¼ ; ð1Þ
2Ma2eff
where M is a translational mass, and aeff is an effective dot radius
given by
aeff ¼ a  gaB : ð2Þ
Here, a, aB, and g are the dot radius, exciton Bohr radius, and the
dead layer coefficient [22], respectively; the QDs are assumed to be
perfectly spherical. With M = 2.3 m0, is aB = 0.7 nm, and g = 0.5, and
the exciton bulk energy given (3.218 eV at 77 K), the effective dot
radius and the average dot radius were experimentally as aeff
3.7
nm and a
4.0 nm. However, the latter value will be larger com-
pared to values obtained by the following experiments because
the peak energy of the QD assembly possessing a certain size dis-
tribution does not agree with that of an averaged size when the
exciton’s energy shift obeys Eq. (1).
3.2. XRD measurements
The XRD patterns of the NaCl crystal without and with CuCl
inclusions before annealing are given on Fig. 2(a) and (b),
respectively. In Fig. 2(a), two strong peaks at 2h = 31.76° and
Fig. 1. The PL (thick curve) and absorption (thin curve) spectra of the NaCl single
crystal with CuCl QD inclusions at 77 K.
86 K. Miyajima et al. / Journal of Crystal Growth 490 (2018) 84–88
Fig. 2. XRD patterns of (a) NaCl crystal without CuCl inclusions (b) NaCl crystal with CuCl inclusions before annealing (c) NaCl crystal with CuCl QD inclusions after annealing
(d) the (4 0 0) planes in CuCl QDs. The contribution due to NaCl single crystals was removed by subtracting the reference XRD pattern. The red calculated curve fits the
experimental data for the mean average radius of 3.5 nm.
2h = 66.25° were observed, corresponding to the diffraction in the
(2 0 0) and (4 0 0) lattice planes of NaCl, respectively. Thus, we
concluded that the NaCl matrix is a single crystal, and the cleaved
surface of the sample is the (1 0 0) plane. In addition, in Fig. 2(b),
two new peaks were observed at 2h = 33.10° and 2h = 69.46°.
According to XRD pattern of CuCl powders, these two weak peaks
can be attributed to the (2 0 0) and (4 0 0) lattice planes of CuCl.
Because no other CuCl diffraction peaks were observed, we con-
cluded that CuCl crystallite particles exist in the NaCl single crystal,
and the lattice planes of the CuCl are parallel to those of the NaCl
matrix. This result agrees with the polarization dependence of the
resonant two-photon absorption of the exciton [41]. This is the first
observation of the alignment of the lattice planes of CuCl and NaCl
using XRD. However, because the sample was opaque, it was
concluded that the diffraction peaks of CuCl originated not from
the QDs but from micrometer-sized particles.
The XRD pattern of the NaCl crystal with CuCl QD inclusions
after annealing is shown in Fig. 2(c). The only peak of the CuCl
(4 0 0) plane appeared at the tail of the diffraction pattern of the
NaCl (4 0 0) plane, and its intensity was lower compared to that
of Fig. 2(b) because of reduced CuCl concentration. It was con-
cluded that this diffraction peak was associated with the CuCl
QDs because of its broadened diffraction width. The peaks due to
the other planes of CuCl did not be observed. Although the peak
of the CuCl (2 0 0) plane is expected to be observed, its intensity
is less than that of (4 0 0) plane. Therefore, it is concluded that
the XRD pattern of CuCl of the sample after annealing is the same
as that of the sample before annealing. In other words, the lattice
planes of CuCl QDs are parallel to those of the NaCl crystal. We
extracted the diffraction curve of the CuCl QDs by subtracting the
tail of the NaCl (4 0 0) peak. This is shown in Fig. 2(d), with the cal-
culated curve fitting the experimental result. From this fitting
result, the dot radius was estimated to be 3.5 nm (±0.4 nm). To
the best of our knowledge, the dot sizes of CuCl QDs measured
using the XRD method are reported here for the first time.
Next, the fluctuations of the lattice alignment were investi-
gated. Fig. 3 (a) and (b) show the rocking curves of the NaCl (2 0
0) planes and CuCl (4 0 0) planes for NaCl crystal with CuCl inclu-
sions before the annealing, where the scanned directions were per-
pendicular to each other. The rocking curves of NaCl in the (2 0 0)
plane had several sharp peaks, indicating that sample consisted of
several domains, whereas those of CuCl (4 0 0) planes were
smooth. However, the CuCl (4 0 0) planes were reproduced well
by convoluting Gaussian functions with those of NaCl (2 0 0)
planes, where full width of a half maximum of the Gaussian func-
tion was 0.1° and 0.2°, respectively. In other words, the lattice
planes of CuCl were almost aligned with those of NaCl albeit with
a small fluctuation of the lattice alignment.
3.3. TEM observation
The TEM images of the NaCl crystals with CuCl QD inclusions
are given in Fig. 4(a). The figure clearly indicates that many parti-
cles with a darker contrast compared to its surroundings exist in
the hexagonally shaped material. Because the atomic number of
Cu (29) is larger than that of Na (11), Cu atoms scatter the electron
beam more than Na atoms. Therefore, we concluded that the CuCl
QDs embedded in a NaCl matrix were observed. Under the assump-
tion of all the QDs being perfectly spherical, the dot radii were
obtained from the areas of the QDs. Fig. 4(b) shows the size distri-
bution of the CuCl QDs. The mean radius of 3.0 ± 0.6 nm was
obtained, which was almost consistent with the results of XRD.
In reality, the shape of the CuCl QDs was not spherical but nearly
polygonal. This can be attributed to higher complexity of growing
spherical CuCl inclusions in NaCl crystals compared to a glass
matrix [25]. At the same time, for other samples, we observed
 K. Miyajima et al. / Journal of Crystal Growth 490 (2018) 84–88 87

Fig. 3. Rocking curves for (a) a certain axis of NaCl and for (b) an axis perpendicular to it for NaCl with CuCl inclusions before annealing. The lower and upper traces are for
NaCl (2 0 0) planes and CuCl (4 0 0) planes. The red curves are the result of convolution of the NaCl rocking curves with the Gaussian functions.

Fig. 4. TEM results: (a) images of the NaCl single crystal with CuCl QD inclusions (b) QD size-distribution.

cubic and hexagonal CuCl QDs clearly, as shown in Fig. 5(a) and (b).
The existence of cubic QDs agrees with previous reports [39,40].
From the XRD results, the lattice planes of CuCl QDs were aligned
to those of the NaCl single crystallite matrix, so we expected the
surfaces of the cubic QDs to be parallel to each other. However,
they were not parallel. During the observations, the TEM images
changed gradually as NaCl and CuCl moved or disappeared under
continuous irradiation. In particular, the shape changes of NaCl
began sooner than that of CuCl and ended several seconds later.
Therefore, TEM images acquisition was performed after NaCl stabi-
lization but before the evolution of CuCl. Consequently, the disor-
der of the cubic CuCl QDs resulted from the transformation of the
NaCl single crystal due to the irradiating electron beam. Therefore,
several surface directions of the cubic CuCl QDs could not be
observed, in contrast to expectations of XRD and two-photon
absorption measurements [41]. Thus, the existence of cubic CuCl
QDs open new horizon for expitaxial growth of the nanoparticles
in single crystallite matrices.

4. Summary

We have obtained and analyzed the absorption and PL spectra

for CuCl QDs embedded in NaCl single crystals. We have character-
Fig. 5. (a) TEM images of the NaCl single crystal with CuCl QD inclusions (b) ized the size, shape, and alignment of the lattice planes of the CuCl
Enlarged yellow squared region of (a). QDs embedded in NaCl single crystals using TEM and XRD
88 K. Miyajima et al. / Journal of Crystal Growth 490 (2018) 84–88
techniques. The XRD patterns of CuCl QDs have been obtained for
the first time, which demonstrate the unidirectional alignment of
the lattice planes in the CuCl and NaCl matrix. The mean radius
of QDs estimated from the diffraction curve was 3.5 ± 0.4 nm. In
addition, we have directly observed CuCl QDs in a NaCl matrix
using TEM for the first time. The shape of the QDs was nearly
polygonal, and the existence of cubical QDs was confirmed. Fur-
thermore, the size distribution was obtained under the assumption
that all the QDs were spherical. The mean dot radius of 3.0 ± 0.6
nm was obtained, that agreed well with the XRD data. On the other
hand, from the absorption spectrum, the mean dot radius was esti-
mated to be 4.0 nm. The difference in the mean dot radius esti-
mated from optical measurements and direct TEM measurements
was attributed to the actual dot size distribution.
Our findings are useful for clarifying the process of QD growth
in crystalline matrices. In contrast with the glass matrices, where
the QDs are produced by the diffusion-controlled growth and the
dot size is the only control parameter (increased with tempera-
ture), in a NaCl crystals, the interface diffusion determines both
the size and shape of the QDs. However, further studies of QD
morphology and its changes induced by annealing conditions can
contribute to the better understanding of its growth process.
Finally, the generation of superfluorescence requires precise con-
trol of the size and shape of high density QD assemblies. Therefore,
our findings are significant to elucidate the relationship between
optical phenomena and QD assemblies.
Acknowledgments
We wish to express our gratitude to Professor Tadashi Itoh of
Osaka University for his helpful advice on sample fabrication. We
wish to thank Dr. Kato for his support with TEM observation and
Dr. Tsukada for his support in obtaining XRD patterns. A part of this
work was conducted at Advanced Characterization Nanotechnology
Platform of the University of Tokyo, supported by ‘‘Nanotechnology
Platform” of the Ministry of Education, Culture, Sports, Science and
Technology (MEXT), Japan. In additionm, this research was partially
supported by KAKENHI 26400320 of the Japan Society for the
Promotion of Science.
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