Enhancing Carrier Transport Properties of Melt-grown CsPbBr3 Single Crystals by Eliminating Inclusions

Article abstract of DOI:10.1021/acs.cgd.9b01616

All-inorganic perovskite CsPbBr₃ has attracted intense attentions due to its inspiring optoelectronic properties and excellent stability. Growing large-size single crystals with high quality is vital both for the intrinsic property investigation and the high-performance device fabrication. Here, large-size CsPbBr₃ single crystals (φ 30 mm × 100 mm) were grown by the modified Bridgman method. The surface morphologies of the as-grown CsPbBr₃ single-crystal wafers were characterized by SEM, and inclusions with size of 1-2 μm were observed in the first-time grown crystal (labeled as CPB-1). By adopting a slower growth rate (0.2 mm/h) and cooling rate (5 °C/h) than that of CPB-1, the inclusions were eliminated in subsequent growth (labeled as CPB-2). The hole mobility-lifetime products were measured to be 3.92 × 10^-3 and 1.46 × 10^-2 cm²·V^-1 for CPB-1 and CPB-2, respectively. The carrier mobility of CPB-2 was enhanced 1 order of magnitude from 10.1 ± 0.3 cm²·V^-1·s^-1 (CPB-1) to 101.3 ± 4.2 cm²·V^-1·s^-1 due to the elimination of inclusions. In addition, CPB-2 exhibited excellent α particles detection ability with the optimal energy resolution of 15.1% at -60 V bias. We provide an effective way to enhance the optoelectronic properties and device performance of melt-grown CsPbBr₃ single crystal by preventing the formation of the inclusions.

Full text of DOI:10.1021/acs.cgd.9b01616

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Article
Enhancing Carrier Transport Properties of Melt-grown
CsPbBr3 Single Crystals by Eliminating Inclusions
Peng Zhang, Qihao Sun, Yadong Xu, Xiang Li, Lin Liu, Guodong Zhang, and Xutang Tao
Cryst. Growth Des., Just Accepted Manuscript • DOI: 10.1021/acs.cgd.9b01616 • Publication Date (Web): 06 Mar 2020
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Crystal Growth & Design
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Enhancing Carrier Transport Properties of Melt-grown CsPbBr Single
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Crystals by Eliminating Inclusions
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Peng Zhang, Qihao Sun, Yadong Xu, Xiang Li, Lin Liu, Guodong Zhang, and Xutang Tao*, †
†
‡
‡
†
†
*, †
†State Key Laboratory of Crystal Materials, Institute of Crystal Materials, Shandong University, Jinan 250100, PR China.
‡State Key Laboratory of Solidification Processing, School of Materials Science and Engineering, Northwestern
Polytechnical University, Xi'an 710072, China.
ABSTRACT: All-inorganic perovskite CsPbBr
excellent stability. Growing large-size single crystals with high-quality is vital both for the intrinsic property investigation and the
high-performance device fabrication. Here, large-size CsPbBr single crystals (ɸ 30 mm×100 mm) were grown by the modified
Bridgman method. The surface morphologies of the as-grown CsPbBr single crystal wafers were characterized by SEM, and
inclusions with size of 1~2 μm were observed in the first-time grown crystal (labeled as CPB-1). By adopting a slower growth rate
0.2 mm/h) and cooling rate (5 °C/h) than that of CPB-1, the inclusions were eliminated in subsequent growth (labeled as CPB-2).
3
has attracted intense attentions due to its inspiring optoelectronic properties and
3
3
(
-3
2
-1
-2
2
-1
The hole mobility-lifetime products were measured to be 3.92×10 cm ‧V and 1.46×10 cm ‧V for CPB-1 and CPB-2, respectively.
2
-1 -1
2
-1 -1
The carrier mobility of CPB-2 was enhanced one order of magnitude from 10.1±0.3 cm ‧V ‧s (CPB-1) to 101.3±4.2 cm ‧V ‧s due
to the elimination of inclusions. In addition, CPB-2 exhibited excellent α particles detection ability with the optimal energy resolution
of 15.1% at -60 V bias. We provide an effective way to enhance the optoelectronic properties and device performance of melt-grown
CsPbBr single crystal by preventing the formation of the inclusions.
3
INTRODUCTION
3
large area wafers suggest the CsPbBr bulk crystal with great
potential in photo detection and nuclear radiation detection. From
this point of view, growing large-size single crystal with high
quality is vital both for the intrinsic property investigation and the
high-performance devices fabrication.
3
Halide metal perovskites with the general formula ABX (where
3 3 2 2
A = CH NH (MA), CH(NH ) (FA), Cs; B = Pb, Sn, Ge; and X =
Cl, Br, I) have been showing great potential in the optoelectronic
1
2
devices including solar cells, light-emitting diodes (LEDs),
photodetectors, nuclear radiation detectors,4 and lasers. Such
wide applications were mainly enabled by the unique properties of
halide perovskites, such as large light absorption coefficient,
superb environment stability, high carrier mobility, and long carrier
3
5
Up to now, it is still a challenge to grow large-size, high purity
and good transparency CsPbBr
methods, i.e., melt growth (vertical Bridgman (VB)
electronic dynamic gradient (EDG))
crystallization (inverse temperature crystallization (ITC)
antisolvent vapor-assisted crystallization (AVC) 24-27) were
employed. Though some millimeter size CsPbBr crystals have
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single crystal, though two general
6, 15-18
and
and solution
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9-20
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-8
21-23
diffusion length.
and
Thanks to excellent thermal and moisture stability compared
with that of organic-inorganic hybrid perovskites, the all-inorganic
3
been grown from the solutions by ITC and AVC technique, it is
difficult to grow the centimeter size due to the low solubility of
perovskite CsPbBr
optoelectronic applications.
quantum dots show great performances in laser, LED and detector
as scintillator. For example, perovskite LEDs with
CsPbBr /MABr quasi-core/shell structure were reported with a
narrow green emission and a record EQE that surpasses 20%. The
flexible and highly sensitive X-ray detectors based on CsPbBr
3
have attracted intense attention in
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-10
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The CsPbBr nano particles and
2
1-27
CsBr and PbBr
2
in solvents.
Another issue for the solution-
method arises from the use of a solution medium for crystal growth
which is different from target material, leading to defects in the as-
a
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2
3
2
grown crystal. Due to the above reason, melt method seems more
potential in growing large-size and high quality CsPbBr single
is congruent melting, and the
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7, 11-17
-
1
crystals.
Firstly, CsPbBr
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nanocrystal exhibited a detection limit of 13 nGy∙s which is 400
1
1
melting point (567 °C) is relatively lower than the most developed
detection semiconductors (CdZnTe, 1092~1295°C, CdTe, 1092
times lower than typical medical imaging doses. Additionally,
more recent research shows bulk CsPbBr single crystal possesses
many unique properties, such as large light absorption coefficient
3
2
8-30
°C),
benefiting the growth of large-size crystals. Secondly, the
were handled in vacuum conditions
5
-1 6,12
13
raw materials CsBr and PbBr
2
(10 cm ),
large atomic number (55/82/35), high resistivity
both in synthesis and growth process, which suppressing the
volatilization of raw materials at high temperature effectively.
However, CsPbBr crystals grown from the melts usually suffer
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from the poorer transparency compared with the crystals grown
from solutions. In general, the impurities, the inclusions (second
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14-15
(
(
10 ~10 Ω‧cm),
large and balance mobility-lifetime product
The investigations about the detector performance
single crystal achieved an energy resolution
-4
-3 4,16
10 ~10 ).
show that the CsPbBr
of 3.9% and 3.8% for 122 keV Co and 662 keV Cs γ-ray,
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respectively, which is comparable with the commercial room
phase) as well as the phase transitions on cooling are the underlying
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temperature detector semiconductor CdZnTe. The performance
of the CsPbBr devices can be further enhanced with the orientation
16, 25
affecting factors of these imperfection.
However, there is no
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report about the investigation of the inclusion in CsPbBr
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single
1
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based on its anisotropic carrier transport properties. These
advantages combining with the possibility in the preparation of
crystal up to now.
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Crystal Growth & Design
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In this work, two batches of CsPbBr
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single crystals were grown
Thermal Expansion Coefficient. The thermal expansion
properties of CsPbBr crystal was studied using a Diamond TMA
thermomechanical analyzer manufactured by Perkin Elmer. The
test sample was a directional CsPbBr crystal with a size of
a×b×c=6×4×3 mm . The testing temperature range is from 25 to
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by the modified VB method. The initial grown CPB-1 exhibited a
poor transparency, while the subsequent crystals CPB-2 grown
after optimizing parameters show excellent transparency. The
inclusions in CPB-1 were observed via SEM, and influence of the
inclusions on the carrier transport properties and the α particle
devices performances were studied in detail.
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450 °C, and the heating rate is 5 °C∙min .
Scan Electron Microscope (SEM) and Energy-dispersive X-ray
Spectroscopy (EDS). The SEM and EDS measurements were
performed using a field emission scanning electron microscope
EXPERIMENTAL SECTION
Synthesis of Polycrystalline CsPbBr
and CsBr (5N) purchased from Aladdin Chemistry Co. Ltd were
used as the starting materials for the synthesis of CsPbBr
polycrystals. Stoichiometric mixtures of PbBr and CsBr (the mole
ratio is 1:1) with the total weight of 200 g were loaded into a silica
ampoule. The silica ampoule was then evacuated to 4×10 Pa and
sealed with oxyhydrogen flame. The sealed ampoule was
subsequently transferred to a pit furnace controlled by a
temperature controller (SHIMADEN FP23). Typically, the heating
program of the furnace was set as follows: firstly, slowly heated to
about 600 °C at a rate of 60 °C/h and held there for 24 hours, then
slowly cooled to 30 °C at 20 °C/h. Finally, the orange color
3 2
. High purity PbBr (5N)
(FE-SEM, Hitachi S-4800) with energy dispersive X-ray
spectrometry (EDS, Horiba EMAX Energy EX-350). The
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accelerating voltage was 15 kV. The samples were polished
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CsPbBr
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wafers with the size of a×b×c=4×4×2 mm .
-4
Device Fabrication. Al and Au electrodes were deposited on the
upper and lower surfaces of the CsPbBr samples by thermal
evaporation, respectively. The Al/CsPbBr /Au asymmetric
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electrode structure was obtained for the evaluation of device
performance.
I-V Characteristic Curve. Current–voltage (I–V) curves of the
Al/CsPbBr /Au devices were measured by an electrical properties
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measurement system (Agilent 4155C) with the bias from -100 V to
100 V.
CsPbBr
single crystal growth.
CsPbBr Single Crystal Growth. CsPbBr
grown by a homemade dual temperature zones vertical Bridgman
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polycrystals were obtained which can be used for the
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single crystals were
α Particle Resolution Spectrum. Detection devices were
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illuminated by an un-collimated
Am@5.48 MeV α particle
2
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furnace as reported in our previous work. The upper hot furnace
zone was set to be 600~800 °C, and the cold zone was set to be
00~400 °C. By controlling the temperatures of the hot and cold
zones, the temperature gradient near the solid-liquid interface was
adjusted to 15~30 °C/cm near the melting point. The obtained
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CsPbBr polycrystals with the weight of 200g were transferred into
a silica ampoule. The ampoule was sealed under a vacuum of 4×10
Pa. Then the ampoule was placed into Bridgman furnace and
heated at 580~600 °C for 6 h. Subsequently, the ampoule was
slowly moved downwards towards the cold zone with a rate of
.2~1 mm/h. When the crystallization process finishes, the
source and the pulse shape information was simultaneously
recorded by connecting the preamplifier (ORTEC 142) output to a
high-speed waveform digitizer card. Then the pulse height spectra
as a function of bias voltage were obtained. The signals from the
preamplifier were further amplified and shaped by the amplifier
2
(ORTEC 570) with a gain of 0.5~200 and shaping time of 2 μs. The
-
final signals were subsequently evaluated by a dual 8 K input
multichannel analyzer (Imdetek AMCA-01) and generated the
response spectrum.
4
RESULTS AND DISCUSSION
0
temperature of furnace cooled down to room temperature with a
rate of 5~15 °C/h.
Crystal Growth and Parameters Optimization. Figure 1a shows
the diagram of the homemade Bridgman furnace. The insulator was
constructed with a gold-coated quartz tube which forms a
semitransparent mirror to protect the heat out of the furnace. Thus,
the growing crystal can be directly observed through the insulator,
and the growth parameters can be adjusted in real time during the
crystal growth process. Figure 1b and c show the pictures of the as-
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Crystal Processing Technology. The as-grown CsPbBr crystals
were cut into 2 mm thick wafers using a STX-202A diamond wire
cutting machine. The surface of the wafer was polished with 7000
mesh sandpaper using acetone as lubricant. In the final step, the
residue on the surface of the sample was removed by the washing
of toluene.
grown CsPbBr
parameters. A slower growth rate (0.2 mm/h) and cooling rate (5
C/h) were adopted for CPB-2 (Figure 1c) growth while CPB-1
Figure 1b) adopted a growth rate of 1 mm/h and a cooling rate of
0 °C/h. The dimensions of the both crystals are 30 mm in diameter
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single crystals grown with two typical different
Powder X-ray Diffraction (PXRD). Powder X-ray diffraction
patterns were collected using a Bruker AXS X-ray powder
diffractometer (Cu Kα graphite, λ=1.5406 Å) at room temperature
in 10°~80° range with a step size of 0.04° and a scanning speed of
0.3 sec/step.
°
(
1
and 100 mm in length, the largest ones reported as far as we know.
Though the PXRD (Figure S1) as well as the GDMS (Table S1 and
S2) results indicated that the both crystals were pure orthorhombic
Glow Discharge Mass Spectrometry (GDMS). Element analysis
performed by Glow Discharge Mass Spectrometry (VG900) for 39
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CsPbBr phase with high purity, CPB-2 exhibits better megascopic
elements in CsPbBr
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single crystals. The diameter and thickness of
transparency than that of CPB-1. From the UV-vis-IR
transmittance spectra in Figure 1c, we can see the transmittance of
the CPB-2 (2 mm thickness) exceeded 65% when the wavelength
over 600 nm, and is about 80% in the 1.2~20 μm region which is
the highest value reported. Correspondingly, the values are 60%
and 72% over 600 nm and 1.2 μm for CPB-1 (2 mm thickness),
respectively. CPB-2 reveals higher transmittance in both visible
region and inferred region, further confirms the better transparency
of CPB-2.
the sample were 30 mm and 2 mm, respectively.
Ultraviolet-Visible and Infrared (UV-Vis-IR) Transmittance
Spectra. The optical transmittance spectra were recorded at room
temperature using a U-4001 UV-vis-NIR spectrophotometer from
2
00-3000 nm, and a Spectrum 100 Fourier transform infrared
spectrometer from 2~20 μm. The samples were cut and polished as
described above, and the thickness of the samples for transmittance
measurement were 2 mm.
Generally, the impurities and the inclusions are the two main
factors which affect the transparency of the single crystal. The
former defect used to form the absorption center, while the latter
will form the light scattering center in the semiconductor. In
Differential Scanning Calorimetry (DSC). The phase transitions
of CsPbBr crystal from room temperature to high temperature was
3
studied by DSC 214 Polyma differential scanning calorimeter. The
test temperature ranged from -173 to 450 °C, and the temperature
-1
CsPbBr
size about 0.5 mm (Figure S2) were observed in the cusp of
CsPbBr crystal which were Pb element proven by EDS (Figure
S3). The formation of Pb particles could attributed to the
3
crystal growth process, some particles with silver color in
change rate was 10 °C∙min . The test sample was CsPbBr
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polycrystalline powder, and the test atmosphere was high purity
nitrogen.
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Page 3 of 9
Crystal Growth & Design
decomposition of PbBr
2
under light irradiation or heating.31 Hence,
discovered in the DSC measurement (Figure 1e) clearly. In
addition, CsPbBr crystal exhibits large and anisotropic thermal
expansion efficiencies (Figure 1f and Table S4, about 1.5~7.5×10
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the slow crystal growth rate is conducive to discharging the
impurities. Our multiple crystal growth experiments (Table S3)
also reveal that the impurities favor to segregate to the end of the
crystal with a slow growth rate. The other possible reason
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-1
K ) which may result in cracks in crystal cooling process. Figure
S4a and b show the picture of the as-grown crystal at 180 °C and
cooling down to room temperature in air, respectively. CsPbBr
responsible for the poor transparency of the melt-grown CsPbBr
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single crystals is the complex phase transform cooling down from
high temperature to room temperature which easily produce
structure defects in crystal. CsPbBr crystal transforms from
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cubic (Pm-3m) to tetragonal (P4/mbm) at 130 °C and transforms
to orthorhombic (Pnma) at 88 °C, subsequently which can be
crystal exhibits excellent transmittance at 180 °C and then
transforms to opaque when cooling down to room temperature in
air. As discussed in Table S3, slow cooling rate of less than 10
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°C/h is essential for the crack control of CsPbBr crystal.
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Figure 1. (a) Diagram of the homemade Bridgman furnace. Photographs of as-grown (b) CPB-1 and (c) CPB-2. (d) Comparison of UV-vis-
IR transmittance spectra of CPB-1 (blue line) and CPB-2 (red line) crystal. (e) DSC and (f) thermal expansion properties of CsPbBr crystal.
components of the inclusions in Figure 2a were measured by EDS
(Figure S5). The results show that the content of Pb in the
inclusions is 2.5%~3.5% higher than the stoichiometric CsPbBr
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Characterization of Inclusions. The inclusion, one of the main
crystal defects, usually forms the optical scattering center or charge
trap center in the crystals, deteriorating the optical and electrical
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,
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2-33
properties of the materials.
The generation of the inclusions
indicating that the inclusions are Pb-rich phase. We suspect that the
formation of the Pb-rich second phase arise from the existence of
3
4
was generally attributed to the impurities in the raw materials, or
the constitutional supercooling at the liquid/solid interface caused
by stoichiometric deviation of the solution. To reveal the micro-
the Pb micro-grains due to the decomposition of PbBr
2
in the melt,
31
forming the mixture of Pb-CsPbBr phase in the crystallization
3
mechanism to the opaqueness of CsPbBr
3
crystals, SEM analysis
process. Therefore, high purity raw materials and slow crystal
growth rate are critical to prepare high purity and good
was performed to compare the surface morphologies of CPB-1 and
CPB-2 wafers. As shown in Figure 2a, the polyhedral inclusions
which form the light scattering centers were observed in CPB-1.
transparency CsPbBr
character the inclusions in CsPbBr
further improving the quality of the CsPbBr
the photoelectric performance of the CsPbBr
3
crystals. Notably, it is the first time to
crystal, which is important for
crystal and optimizing
devices.
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The type size of the inclusions is 1~2 μm with a density about 10
3
-2
cm . Figure 2b shows the micro morphology of CPB-2,
demonstrating a clean surface without any inclusions. The
3
Figure 2. SEM images of (a) CPB-1 and (b) CPB-2 with different magnification scales.
Schottky Type Devices and Dark Current. To investigate the account of the low work function of Ga (4.3 eV) and high work
influence of the inclusions on the electronic properties of CsPbBr
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function of Au (5.1 eV). However, considering the poor
single crystal, the I-V characteristics of the devices prepared with
CPB-1 and CPB-2 were measured for comparison. The appropriate
electrode design can realize the Schottky junction which restrains
penetration ability of α particles, the painted Ga electrode is too
4
thick to be penetrated completely by α particles. Therefore, Al
electrode with the same work function (4.3 eV) with Ga and better
electric conductivity was selected in the electronic property
measurements in this work. Figure 3a is the schematic diagram of
3
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the leakage current significantly. In the previous reports, Ga and
Au asymmetric electrodes were brushed on CsPbBr crystal to form
the Schottky device which reduce the dark current dramatically on
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the Al/CsPbBr /Au device. The thickness of the CsPbBr wafer is
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Crystal Growth & Design
Page 4 of 9
2
mm, and the size of electrode is 100 nm in thickness and 4×4
under positive bias was attribute to the higher purity of the
materials and the less second phase in the crystal. The inset of
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mm in square. Figure 3b shows the energy level diagram of this
device. Figure 3c and d are the I-V curves of the devices based on
CPB-1 and CPB-2 under continues bias from -100 V to 100V,
respectively. For CPB-1, the dark current of the device was about
Figure 3c and d show the I-V curves in the negative voltage range
which indicate impressive rectification effect for both CPB-1 and
CPB-2 with the dark current only 26 nA and 7.5 nA, respectively.
The dramatic decrease of dark current of the detector based on
2
14 nA under 100 V bias. In contrast, it was about 93 nA under 100
16
V bias for the CPB-2 device. The lower dark current of CPB-2
CPB-2 results in low detector operation noise.
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Figure 3. (a) Schematic illustration of the Al/CsPbBr
of the device based on (c) CPB-1and (d) CPB-2.
3
/Au device. (b) Energy level diagram of the Al/CsPbBr
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/Au device and Dark current
α Particle Resolution Spectrum and Carrier Transport
Properties. Figure 4a illustrates the diagram of the carrier transport
Bias (V)
FWHM
110
99
Resolution
24.6%
21.2%
19.8%
17.8%
16.7%
15.1%
-10
20
2
41
process of CsPbBr
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crystal irradiated by
Am@5.48 MeV α
-
particles. Under the irradiation of α particles, electron and hole
pairs generated near the Al anode, and they separated and drifted
to Al anode and Au cathode driven by the external electric field,
-30
40
95
-
86
3
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respectively. The penetration depth can be calculated by the
-50
-60
81
3
7-38
Bragg-Kleeman rule:
푅 = 퐴퐸푃
74
a
(1)
(2)
Note that the full-energy peaks shift to higher channel with
increasing the applied bias for α particles detection. Based on the
relationship between the position of the peaks and the applied bias
푀푅a
푅 = 0.00032 ×
휌
a
where R is the range in cm of an α particle in standard air, A and P
h
voltages, the hole mobility-lifetime product (μτ) of CPB-1 and
CPB-2 were fitted using the single carrier Hecht equation:
is a constant (A=0.325 and P=1.5 for the energy of 4~8 MeV α
particle), E is the energy of α particle, R is the required range in the
sample, M and ρ is the atomic weight (579.82) and density (4.84
2
휇휏푉
―푑
푄/푄 =
1 ― exp(
)
(3)
0
푑2
[
]
휇휏푉
3
g/cm ) of the sample, respectively. Different with the interaction
between γ-rays and semiconductors, in which the γ-rays can
penetrate into the deep depth of the bulk crystals, the penetration
where Q is the channel of the full-energy peak, Q is the theoretical
0
number of saturated channels per peak, V is the applied bias and d
is the thickness of the sample. The calculated (μτ) for CPB-1 was
depth of α particles into the CsPbBr
3
crystal is calculated to be ~64
h
μm which is negligible compared to the thickness (2 mm) of the
-
3
2
-1
-2
2
-
3
1,
.92×10 cm ‧V , and the value for CPB-2 was 1.46×10 cm ‧V
4
single crystal detector.
3 times larger than that of CPB-1. The higher (μτ) of CPB-2
h
Figure 4b and d show the induced pulse height spectra as the
function of applied bias (-10~-60 V) for CPB-1 and CPB-2
detectors, respectively. Based on the suitable Schottky structure of
should attribute to the elimination of the inclusions which traps or
scatters the carrier, deteriorating the resolution and the response of
32, 34, 39
the devices.
In addition, the (μτ)
h
for both CPB-1 and CPB-
3
Al/CsPbBr /Au and high purity of CPB-2, the sharp full-energy
2
3
are much higher than that of many halide perovskites (MAPbI ,
peaks with low noise were well resolved on the α particles detection
spectrum of CPB-2 detector, while the CPB-1 exhibited a poor
performance. The full width at half maximum (FWHM) and energy
resolution under different bias for CPB-2 were summarized in
-2
2
-1
-4
2
-1 40, 41
(μτ)
e
=1.0×10 cm ‧V and MAPBr
3
, (μτ)
e
=2.2×10 cm ‧V )
-5
-4
2
-1 16
and commercial CdZnTe ((μτ) =10 ~10 cm ‧V ), except for
h
FAPbI
3
(1.8×10-2 cm2 ‧ V-1).40 The high μτ product of CsPbBr
3
241
Table 1. The optimal resolution of 15.1% for Am@5.48 MeV α
crystal implies the wonderful prospect in photoelectrical and
radiation detection.
particles under -60 V bias is comparable to the reported value of
4
3
CsPbBr crystal detector.
Table 1. FWHM and resolution of the detector based on CPB-2.
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Crystal Growth & Design
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Figure 4. (a) Diagram of the carrier transport process irradiated by α particles. 241Am α particle spectrum under negative voltage of (b) CPB-1
and (d) CPB-2. Mobility-lifetime product fitted based on Hecht equation for (c) CPB-1 and (e) CPB-2.
Figure 5a and c show the transient pulses of hole transport of the
devices based on CPB-1 and CPB-2 under negative bias,
respectively. The preamplifier signals were collected to obtain the
carrier drift time (tdr), and we can see the average rise time decrease
with the increase of the bias voltage from -10 V to -70V. Figure 5b
and d show the carrier drift velocity as the function of the electrical
field (vdr) for CPB-1 and CPB-2, respectively. The carrier mobility
μ was calculated using the expression:
V-1
‧s-1 for CPB-1 and CPB-2, respectively. Compared with the
CPB-1, the hole mobility of CPB-2 enhanced about one order of
magnitude, which implies the elimination of the inclusions reduce
the scattering center and benefit the carrier transport performance
3
of CsPbBr crystal.
Due to the different crystal growth technique and measurement
methods, great contradiction in the reported carrier mobility of
CsPbBr
푑2
3
exited. As listed in Table 2, the carrier mobility of
푣dr
휇 = 퐸 = 푉푡dr
(4)
CsPbBr single crystal is varied in a wide range about 10~2000
3
2
-1 -1
cm ∙V ∙s in the last 6 years’ reports. By eliminating the inclusions
in CsPbBr crystal and adopting a reliable measurement technique,
where E is the electric field intensity, d is the thickness of the
3
sample and V is the applied voltage. The hole mobility μ
1
and μ
2
our work revealed the hole mobility of CsPbBr
intrinsic property.
3
closer to the
2
-1 -1
2
fitted from the data were 10.1±0.3 cm ‧V ‧s and 101.3±4.2 cm ‧
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9
0
Figure 5. Induced α pulse shapes at different negative voltages of (a) CPB-1 and (c) CPB-2. Carrier drift velocity as function of the electrical
field of (b) CPB-1 and (d) CPB-2.
3
Table 2. Comparison of carrier mobility of different CsPbBr single crystals.
2
-1 -1
2
-1 -1
Growth method
VB method
AVC
VB method
ITC
Measurement method
μ
e
(cm ∙V ∙s )
μ
h
(cm ∙V ∙s )
Ref.
[
[
[
15]
25]
16]
TOF
Hall
TOF
1000
143
-
52
13.6
2300
11.61
-
52±1
11
[21]
[24]
SCLC
SCLC
TOF&SCLC
SCLC
TOF
AVC
[6]
VB method
VB method
VB method
VB method
2000
-
10.1±0.3
101.3±4.2
[17]
This
work
TOF
-
CONCLUSIONS
In this work, inorganic perovskite CsPbBr
the dimensions of 30 mm in diameter and 100 mm in length, the
largest crystals reported as far as we know, were grown by
ASSOCIATED CONTENT
Supporting Information. This material is available free of charge
via the internet at http://pubs.acs.org.
Figure S1. PXRD of the CPB-1 and CPB-2.
3
single crystals with
modified Bridgman method. The micro morphology of CsPbBr
3
Figure S2. Pb particle with silver color in size about 0.5 mm in the
single crystal was characterized by SEM, and the polyhedral
inclusions were observed in CPB-1 for the first time. The
inclusions were eliminated in CPB-2 with a slower growth rate (0.2
mm/h) and cooling rate (5 °C/h) than that of CPB-1. The measured
cusp of CsPbBr
Figure S3. EDS of the particle with silver color in the cusp of
CsPbBr crystal.
Figure S4. (a) Photograph of the as-grown CsPbBr
3
crystal.
3
3
crystal which
crystal
-3
2
-1
-2
(
h
μτ) for CPB-1 and CPB-2 were 3.92×10 cm ‧V and 1.46×10
putted forward at 180 °C. (b) The picture of the CsPbBr
after cooling down to room temperature in air.
Figure S5. EDS of the inclusion in CPB-1.
3
2
-1
cm ‧V , respectively. Correspondingly, the hole mobility was
improved from 10.1±0.3 cm ‧V ‧s (CPB-1) to 101.3±4.2 cm ‧V
2
-1 -1
2
-
1
-1
‧s
(CPB-2), one order of magnitude large. The α particle
Table S1 and 2. GDMS of CPB-1 and CPB-2, respectively.
Table S3. CsPbBr single crystals grown by modified VB method
resolution spectrum collected by the detector based on CPB-2
showed an optimal energy resolution of 15.1% at -60 V bias. The
prevention of the inclusions is an efficient way to enhance the
3
with different crystal growth parameters.
Table S4. Thermal expansion coefficient of CsPbBr crystal.
3
3
photoelectric properties for CsPbBr single crystal.
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Crystal Growth & Design
Haghighirad, A. A.; Moore, D. T.; Snaith, H. J. Bandgap-Tunable
Cesium Lead Halide Perovskites with High Thermal Stability for
Efficient Solar Cells. Adv. Energy Mater. 2016, 6, 1502458.
AUTHOR INFORMATION
Corresponding Author
(X.T.) E-mail: txt@sdu.edu.cn
(G.Z.) E-mail: zgd@sdu.edu.cn
1
2
3
4
5
6
7
8
9
(11) Chen, Q.; Wu, J.; Ou, X.; Huang, B.; Almutlaq, J.;
Zhumekenov, A. A.; Guan, X.; Han, S.; Liang, L.; Yi, Z.; Li, J.;
Xie, X.; Wang, Y.; Li, Y.; Fan, D.; Teh, D. B. L.; All, A. H.;
Mohammed, O. F.; Bakr, O. M.; Wu, T.; Bettinelli, M.; Yang, H.;
Huang, W.; Liu, X. All-inorganic perovskite nanocrystal
scintillators. Nature 2018, 561, 88-93.
(12) De, Roo J.; Ibáñez, M.; Geiregat, P.; Nedelcu, G.;
Walravens, W.; Maes, J.; Martins, J.; Driessche, I.; Kovalenko, M.;
Hens, Z. Highly dynamic ligand binding and light absorption
coefficient of cesium lead bromide perovskite nanocrystals. ACS
Nano 2016, 10, 2071-2081.
ORCID
Guodong Zhang: 0000-0002-9048-9270
Xutang Tao: 0000-0001-5957-2271
Author Contributions
All authors have given approval to the final version of the
manuscript.
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Notes
(
13) Liu, X.; Xu, T.; Li, Y.; Zang, Z.; Peng, X.; Wei, H.; Zha,
W.; Wang, F. Enhanced X-ray photon response in solution-
synthesized CsPbBr nanoparticles wrapped by reduced graphene
oxide. Sol. Energy Mat. Sol. Cells 2018, 187, 249-254.
14) Zhang, M.; Zheng, Z.; Fu, Q.; Guo, P.; Zhang, S.; Chen, C.;
Chen, H.; Wang, M.; Luo, W.; Tian, Y. Determination of Defect
Levels in Melt-Grown All-Inorganic Perovskite CsPbBr Crystals
The authors declare no competing financial interest.
3
ACKNOWLEDGMENT
This work was supported by the National Key Research and
Development Program of China (Grant No. 2016YFB1102201),
the National Natural Science Foundation of China (Grant No.
(
3
by Thermally Stimulated Current Spectra. J. Phys. Chem. C 2018,
122, 10309-10315.
(15) Stoumpos, C. C.; Malliakas, C. D.; Peters, J. A.; Liu, Z.;
Sebastian, M.; Im, J.; Chasapis, T. C.; Wibowo, A. C.; Chung, D.
Y.; Freeman, A. J.; Wessels, B. W.; Kanatzidis, M. G. Crystal
5
1972194, 51932004, 61975098), Program of Introducing Talents
of Disciplines to Universities in China (111 program No.
BP2018013), the Fundamental Research Funds of Shandong
University, the Shandong Provincial Key Research and
Development Program (Grant NO. 2018GGX102003)
Growth of the Perovskite Semiconductor CsPbBr
3
: A New
Material for High-Energy Radiation Detection. Cryst. Growth Des.
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Crystal Growth & Design
Enhancing Carrier Transport Properties of Melt-grown CsPbBr Single Crystals by Eliminating Inclusions
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and Xutang Tao*, †
Peng Zhang, Qihao Sun, Yadong Xu, Xiang Li, Lin Liu, Guodong Zhang,
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CsPbBr
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single crystals (CPB-1 and CPB-2) were grown by modified Bridgman method with different technique parameters. The
polyhedral inclusions were observed in CPB-1 for the first time via SEM. And the inclusions were eliminated in CPB-2 by optimize the
crystal growth parameters. Correspondingly, the hole mobility was improved from 10.1±0.3 cm ‧V ‧s (CPB-1) to 101.3±4.2 cm ‧V ‧s
CPB-2), one order of magnitude large.
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