Visual clarity methylammonium lead trichloride perovskite single crystals for X and gamma rays protection

Article abstract of DOI:10.1016/j.jallcom.2019.151896

Ionization radiation photons such as X-ray and gamma ray have been widely applied in the nuclear power industry, medical imaging, scientific research, and aerospace exploration. Developing a protective material with excellent shielding properties and clear visibility is an urgent demand in order to protect people who are working in a radiation environment. Hence, we present a highly efficient radiation shielding material based on lead halide organic-inorganic perovskite single crystals with visual clarity, high efficiency and attenuation coefficient, and thin half-value layer. Our results indicate that the shielding performances (mass attenuation coefficients, effective atomic numbers and half value layer) of the perovskite crystals are at least one order higher than the current commercial products, such as Bone-equivalent plastic, Polyethylene terephthalate, and colorless glass. In addition, physical properties (density), and optical properties (transmission, refractive index), can be slightly tuned by the dopant Br concentration in crystals. The present results demonstrate that the organic-inorganic perovksite single crystals are optimized for high attenuation radiation shielding materials with visual clarity.

Full text of DOI:10.1016/j.jallcom.2019.151896

Journal Pre-proof
Visual clarity methylammonium lead trichloride perovskite single crystals for X and
gamma rays protection
Qiang Xu, Wenyi Shao, Yang Li, Hang Zhang, Xiao Ouyang, Xinlei Zhang, Jing Nie,
Xiaoping Ouyang, Bo Liu
PII:
S0925-8388(19)33135-4
DOI:
https://doi.org/10.1016/j.jallcom.2019.151896
JALCOM 151896
Reference:
To appear in: Journal of Alloys and Compounds
Received Date: 24 June 2019
Revised Date: 12 August 2019
Accepted Date: 15 August 2019
Please cite this article as: Q. Xu, W. Shao, Y. Li, H. Zhang, X. Ouyang, X. Zhang, J. Nie, X. Ouyang,
B. Liu, Visual clarity methylammonium lead trichloride perovskite single crystals for X and gamma rays
protection, Journal of Alloys and Compounds (2019), doi: https://doi.org/10.1016/j.jallcom.2019.151896.
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Graphical Abstract

Visual clarity methylammonium lead
trichloride perovskite single crystals for X
and Gamma rays protection
Qiang Xu, a,* Wenyi Shao, a Yang Li, a Hang Zhang, a Xiao Ouyang, b Xinlei Zhang, a
Jing Nie, a Xiaoping Ouyang, a,b,c and Bo Liu d
aDepartment of Nuclear Science and Engineering, Nanjing University of Aeronautics
and Astronautics, Nanjing 211106, China
bCollege of Physics, Institute of Nuclear and New Energy Technology, Tsinghua
University, Beijing, 100084. Beijing, China
c Northwest Institute of Nuclear Technology, Xi’an, 710024, China
dSchool of Physics Science and Engineering, Tongji University, Shanghai 200092,
China
*Corresponding author: xuqiangxmu@nuaa.edu.cn (Q.X)
ABSTRACT
Ionization radiation photons such as X-ray and gamma ray have been widely applied in
the nuclear power industry, medical imaging, scientific research, and aerospace
exploration. Developing a protective material with excellent shielding properties and
clear visibility is an urgent demand in order to protect people who are working in a
radiation environment. Hence, we present a highly efficient radiation shielding material
based on lead halide organic-inorganic perovskite single crystals with visual clarity,
high efficiency and attenuation coefficient, and thin half-value layer. Our results
indicate that the shielding performances (mass attenuation coefficients, effective atomic
numbers and half value layer) of the perovskite crystals are at least one order higher
than the current commercial products, such as Bone-equivalent plastic, Polyethylene
terephthalate, and colorless glass. In addition, properties, physical properties (density),

and optical properties (transmission, refractive index), can be slightly tuned by the
dopant Br concentration in crystals. The present results demonstrate that the
organic-inorganic perovksite single crystals are optimized for high attenuation radiation
shielding materials with visual clarity.
Keywords: Perovskite single crystals, Radiation shielding, X-ray protection,
Gamma-ray protection, High attenuation coefficient
1. Introduction
Radiation photons (X-ray or gamma ray) have been employed as valuable tools in
medical, agriculture, scientific research, homeland security and aerospace exploration
[1-6]. While all these applications are greatly helpful for human life, unwanted
exposures such as scattering X-rays, emergency accidents and cosmic ray are
hazardous to lives with varying effects. High dose radiation can produce immediate
harmful effects, such as skin burn, radiation sickness, and radiation can increase the
risk of cancer [7,8]. Therefore, how to prevent radiation that could cause physical
harm to human and their surroundings is a serious safety concern to use that
equipment, which potentially emits hazardous rays [9,10].
The incident photons either scattered or absorbed in a single event through various
interaction process with atoms, electrons or nuclei of materials [11]. Thus, high
atomic number (Z) materials have been employed to attenuate the X-ray or gamma
ray. In general, metallic shielding materials with a high density such as iron (Fe), lead
(Pb), tungsten (W) are effective alternatives for reducing the intensity of radiation.
Among those heavy metallic materials, Pb is traditionally the most popularly and
widely material used for providing durable shielding of gamma rays and X-rays, due
to its high atomic number and easy process. However, these heavy and bulky metallic
materials could not serve all the requirements of most applications [12]. For example,
mobile nuclear devices and manned space crafts, lightweight and have less volume
radiation shielding materials are preferred due to space and maneuverability

constraints imposed by the vehicles. In addition, in medical and scientific research,
optically clear with full radiation protection is suitable for observation windows to
protect observers, operators, or workers [13].
Recently, numerous research focuses on lead-based shielding materials with
transparent in visible light for shielding the unwanted X or gamma radiation. Lead
glass and polymer are the most successful commercial products for X(γ) ray shield.
Lead glass is heavy, expensive and easily breakable, the density of the polymer is low
and with weak attenuation performance. In addition, the shielding efficiency of those
materials is lower than the theoretical expectation, especially when they are thin [14].
Therefore, there are still some challenges that limit their applications such as cost,
weight and optical properties (refractive index, nonlinear optical susceptibility,
infrared transparency) [15]. Much efforts still seek to develop new shielding materials
with low cost, high attenuation coefficients, the visible light transparent and other
specific physical properties that can reduce as much as possible harmful X or gamma
rays to meet the particular safety requirement [10-15]. A visual clarity shielding
material is expected to have high transparent, high attenuation coefficients and thin
half value layer that can significantly attenuate the incident radiation intensity with
relatively small materials.
Organic-inorganic methylammonium lead halide perovskite materials CH3NH3PbX3
(MAPbX3, where MA is CH3NH3, X=Br, I, Cl) have been attracted in a variety of
optoelectronics applications such as solar cell, light emitting diodes (LEDs), laser and
photodetectors [16-19]. The outstanding performances of these applications are
mainly attributed to the electronic properties (high mobility–lifetime product, long
diffusion length and low trap density) and optical properties (high absorption
coefficient, tunable direct optical band-gap) [20-22]. In addition, thanks to the
existence of heavy atoms enhanced the ionization radiation attenuation properties,
perovskite also has been successfully demonstrated to detect ionization radiation
(charged particles, X(γ) ray) [23-26]. Therefore, perovksite materials are optimal for
radiation shielding.
In this paper, we have successfully grown a high quality visible light transparent

MAPbBrxCl3-x SCs with various dopant concentration and thickness by using the
solution growth method. These organic-inorganic perovskite materials exhibit high
transparent and attenuation coefficients with high effective radiation shielding
performance. The shielding performance for 59keV photons is more than 10 times
higher than that of polymer composites [27-29].
2. Experimental section
2.1 Synthesis of perovskite single crystals
Synthesis of perovskite single crystals: High quality perovskite single crystals were
synthesized by using inverse temperature crystallization growth method with two
steps. Firstly, growth CH3NH3Cl (MACl) powder using a molar ratio of 1:1
methylamine (33 wt% in absolute ethanol) and hydrochloride acid (33 wt% in water)
stirred at 0℃ ice bath for 1.5 h. To increase the purity, the raw, as-grown MACl
powder was washed with ethanol and diethyl ether for at least three times, until it
appears snow white. Then, prepare precursor solution by dissolving various molar
ratios of MACl, PbBr2 (99.99%), PbCl2 (99.99%) into 2 mol dimethyl sulfoxide
(DMSO, 99%) until it saturated. A 2µm PTFE filter was used to filter the precursor
solution, and then semi-transparent high-quality Br-doped MAPbCl3 SCs were
harvested from solution after increasing its temperature to 90 ℃. The size of the
crystal was determined by the growth time.
2.3. Characterization
The element's content of crystals was characterized by a homemade X-ray
fluorescence (XRF) spectroscopy system at room temperature. This system consists of
X-ray tube, a silicon drift detector (Amptek XR-100SDD) with a Be window and a
laser rangefinder. Optical transmission spectrum was recorded using a Cary 5000
UV-Visible spectrometer in the range of 350-600nm.
The radiation shielding performances were recorded by a radiation dosimeter and
spectroscopy detection system. The pulse height spectrum was recorded by a High
purity Germanium (HPGe) detector from ORTEC inc. X-ray photons were coming
from X-ray tube (Mo target) operated at a various voltage, which collimated by a

copper collimator with the diameter of 2mm. Am-241 (0.25µCi) and Pu-238 (8.79mCi)
were employed as excited γ ray radiation source. To avoid the effect of emitted alpha
particles from the Am-241 source, a thin layer of 0.5mm Teflon was covered on the
radiation surface. All the measurements were in air at room temperature.
3. Results and discussion
3.1. Materials characterization
Fig. 1. Physical properties of MAPbBrxCl3-x SCs. (a) side view of three
MAPbBrxCl3-x SCs with different thickness and Br dopant concentration. (b)
calculated effective Z value of crystals with various Br content. (c) the density of
MAPbBrxCl3-x SCs as a function of Br concentration. (d) XRF spectra of
MAPbBrxCl3-x SCs that excited by 25keV X-ray from a portable X-ray tube with a
silver anode, operated at 25kV. The black triangle stands for Cl element, the red
square stands for Pb element, the blue circle stands for Br element. This measurement
is carried in the air at room temperature, thus the signals from the air and background
shielding materials have been recorded.
Various semi-transparent Br dopant MAPbCl3 SCs with different thickness have been
harvested from the saturated dimethyl sulfoxide (DMSO) solution (Materials and

growth method) that consists of MACl, PbCl2 and PbBr2. The color of the crystals is
determined by the Br concentration, the real optical images of MAPbBrxCl3-x SCs as
shown in Figure 1a. Effective atomic number (Zeff) and density are two basic physical
parameters that indicate the radiation shielding properties. High Zeff and density are
the two key strategies to obtain excellent shielding performance for X (γ) ray. Zeff is
ꢅ.ꢆꢇ
ꢄ
∑
theoretically given by using Mayneord’s equation Zꢀꢁꢁ
=
ꢃ nꢃZꢃ , where, nꢃ is
ꢂ
the relative fraction of the total number of electrons, Zꢃ is the atomic number of each
element [30]. The density of the crystals is measured from the real crystals. The Zeff
and density values are tuned from 66.6 and 3.0g/cm3 to 83.7 and 3.79 g/cm3 with the
increasing of heavy atomic Br concentration (as shown in Figure 1b and 1c). To
measure the Br concentration, we have investigated the crystals by using a homemade
X-ray Fluorescence (XRF) analysis system [31]. Three main peaks ascribed to Pb, Cl
and Br elements have been observed, the other peaks are from air and/or the
background shielding materials. The actual molar ratio of Cl/(Cl+Br) in
MAPbBrxCl3-x SCs is obtained from these three peaks (Table 1).
Table 1 the chemical composition of MAPbBrxCl3-x
Pb wt%
58.19
50.36
51.20
51.89
52.26
52.76
Cl wt%
41.81
48.22
44.96
42.82
40.34
39.10
Br wt%
0
MAPbCl3
MAPbBr0.04Cl2.96
MAPbBr0.11Cl2.89
MAPbBr0.16Cl2.84
MAPbBr0.23Cl2.77
MAPbBr0.25Cl2.75
1.42
3.84
5.29
7.4
8.14

3.2 Optical properties
Fig. 2. Tunable optical properties of MAPbBrxCl3-x SCs. (a) normalized transmission
of MAPbBrxCl3-x SCs in the range of 350 nm to 600 nm; (b, c) calculated optical
band-gap and refractive index versus molar ratio of Cl/(Br+Cl).
Optical characterizations (transmission, optical band-gap and refractive index) of the
MAPbBrxCl3-x SCs are presented in Figure 2. Transmission spectra were carried out at
room temperature by Cary 5000. The transmission of the crystals are depended by the
thickness. Sharp and clear cut-off edges have been observed that tunable with the
dopant Br content, which is attributed to band-gap absorption. Optical band-gap was
extracted from the cut-off edge by using Tauc’s equation. The relationship between
optical band-gap and the molar ratio of Cl to Br+Cl is plotted in Figure 2b, that
exhibits a nearly linear relationship with the increasing of Cl content from 2.18eV of
MAPbBr3 to 3.0 eV of MAPbCl3. Refractive index is an important metric that
determines the path of a visible photon at the interface at two media, and also
correlates to the band-gap. The refractive index product is obtained using Moss
equation: Eꢈnꢉ = k, where k is a constant with a value of 108eV [32,33]. Figure 2c
shows the calculated refractive index as a function of molar ratio, at a low content of
Br, and the refractive index at around 2.3 has been obtained. With the increasing of Br
content, refractive index is decreasing to about 1.6. The results indicate that the
optical properties (transmission, optical band-gap and refractive index) of
MAPbBrxCl3-x SCs are strongly dependent by the concentration of dopant Br.

3.3 X- and Gamma rays shielding
Fig. 3. Radiation shielding: (a) schematic of the experiment for radiation shielding
measurement. (b) typical pulse height spectra distribution of γ ray that shielded by
MAPbCl3 SCs samples. The spectra were collected by High purity Germanium
detector. The radiation source is Am-241 with the activity of 0.25 µCi. (c) radiation
shielding efficiency of X-ray as a function of dopant Br and incident X-ray energy.
To measure the X(γ) ray shielding properties of the crystals, the schematic of our
homemade measurement is shown in Figure 3a. It consists of a radiation source, lead
collimator, and dosimeter or radiation detector. The radiation source of X-ray from an
X-ray tube with Ag target and γ ray from radioactive isotope source, respectively. All
radiation sources were collimated by a lead collimator with a diameter of 2mm. The
shielding perovskite crystals were placed between collimator and detector with the
same height. High purity Germanium (HPGe) detector and X(γ) ray dosimeter were
employed to investigate the attenuation performance.
Figure 3b shows the pulse height spectra of Am-241 radiation source with and without
shielding. To avoid the effect of the charged particles, a thin layer of white paper has
been used to cover the surface of the source. When a thin MAPbCl3 SCs with the
dimension of 10.18mm (L)×11.2mm (W)×0.54mm (H) was employed to shield the
59keV γ-ray from the source, the intensity of photopeak is decreased several times.
Furthermore, an X-ray tube with Mo target has been employed as a radiation source
that operated at a different voltage. The dimension of the other two samples
MAPbBr0.02Cl2.98 and MAPbBr1.65Cl1.35 are 9.6 mm (L)×9.7 mm (W)×0.49mm (H)
and 10.43 mm (L)×11.55 mm (W)×0.35mm (H), respectively. These three samples

presented good shielding efficiency, as shown in Figure.3c. The shielding efficiency is
defined as (1-I/I0)×100%, where, I is the initial radiation intensity, I0 is the transmitted
radiation intensity. The shielding efficiency is decreasing, while the energy of incident
X-ray is increasing. The best shielding efficiency of these three samples is up to 90%,
while the X-ray tube operated at 30kV.
Fig. 4. (a) Mass attenuation coefficient and (b) half value layer of MAPbCl3 with
different dopant Br concentration, and as a function of photon energy.
It is worthwhile to be mentioned that the radiation shielding efficiency decreased with
the Br doped into the perovskite SCs, this is ascribed to the different thickness of
these three samples. Thus two precise metrics are used to evaluate the radiation
μ
shielding performance: mass attenuation coefficients ( ꢊ ) and half value layer (HVL).
ρ
For a non-radiation scattering attenuation medium, according to Beer-Lambert’s law
ꢎ
μ
equation,I = Iꢋeꢌꢍ ꢊ ꢐꢏꢑ , where ꢊ is the mass attenuation coefficient, ρ is the
ꢏ
ρ
density of material, I is the intensity of incident radiation photons and Iꢋis the
intensity of transparent radiation photons, and x is the thickness of the material. HVL
is defined as the thickness of the materials at which the incident radiation intensity is
0.693
reduced by one half. It is can be calculated from the equation of HVL =
ꢊ .
μ
To measure these two important metrics, a series of radioisotopes (Am-241: 59keV;
Pu-238: 43keV, 99keV, 152keV;) have been used as gamma source. The values of
μ
ꢊ and HVL for various Br dopant MAPbCl3 SCs have been measured as shown in
ρ
μ
Figure 4. It is observed that the value of ꢊ is increasing with the Br concentration,
ρ

which is due to the higher density of crystals with more Br concentration than that of
μ
pure MAPbCl3 single crystals. The ( ꢊ ) values are decreasing with the increasing of
ρ
incident radiation photon energy, due to the weak attenuation efficiency. However, the
μ
values of ( ꢊ ) exhibit a weak increasing at 100keV comparing with 59keV, this is
ρ
because of the X-ray absorption resonance at the electronic edge of Pb K shell in
MAPbBrxCl3-x.
Table 2 Comparison of perovskite materials with comercial shielding materials at
59keV
Density
µ/ρ
HVL
Materials
(Zeff) transparency
Ref
(g/cm3) (cm2/g) (cm)
Error
!
Refer
ence
sourc
e not
found
.[27]
Error
!
Bone-equivalent
plastic (B-100)
1.45
0.253* 1.89*
7.57
clarity
Refer
ence
sourc
e not
found
.[27]
Polyethylene
terephthalate
(mylar)
1.38
0.175* 2.87*
4.6
clarity
Al–steel
1.9-
2.0
2.7
0.711
0.277
0.55
0.92
21.4
11.7
opacity
opacity
[28]
composite foam
Aluminum A3 56
Error

!
Refer
ence
sourc
e not
found
.[28]
Steel–steel
2.7-2.8
0.92
0.28
26.8
opacity
clarity
clarity
[28]
[29]
composite foam
1.80-
2.03
0.391- 0.714- 13.55-
Colourless glass
MAPbBr0.25Cl2.75
0.478
6.1
0.977 15.05
0.03 83.7
This
3.79
paper
*Calculated result from the literature
We then compared the shielding performances of the perovskite materials with
successful commercial products (polymer, plastic, glass). As shown in Tabel 2, our
results indicate that the shielding ability of perovksite is about 10 times or more than
Bone-equivalent plastic (B-100), Polyethylene terephthalate (mylar) [27], plastic [28],
colourless glass [29].
Fig. 5. Schematic of shielding process: (a) photoelectric effect process, electrons are
emitted from atoms; (b) proposed mechanism of X (γ) interaction with MAPbBrxCl3-x
at low energy (<500keV). When a beam of X (γ) ray pass through the crystals and
collides with heavy atoms (Pb, Br, Cl), it will transfer all of its energy to the eject

electron. Therefore, the incident X (γ) rays are attenuated by perovskite materials.
The shielding performances of perovskite materials are correlated to the interaction with
incident ionization photons (X or γ ray). A beam of ionization photons exposure onto the
materials, three main physical processes can occur while these photons interact with the
materials: the photoelectric effect is the emission electrons from atoms; Compton scattering is
the scattering of photons on electrons resulting energy loss; pair production is the absorbed
photons created an electron-positron pairs near a nucleus. Thus, the total attenuation
coefficients(μꢒꢓꢒꢔꢕ) can be expressed as [34]:
ꢖꢗꢘꢗꢙꢚ = ꢖꢛꢜ + ꢖꢝꢘꢞꢛ+ꢖꢛꢙꢟꢠ
(1)
where, μꢡꢀ, μꢢꢓꢣꢡ, and μꢡꢔꢃꢤ are the attenuation coefficients caused by photoelectric effect,
Compton scattering, and pair production, respectively. For a given material, the interaction
mechanism between photons and material are depended by incident photons energy. At low
energy (<500keV), photoelectric absorption is the dominant process. As shown in Figure 5,
the incident photon is completely absorbed by atomic and transfer its energy to the electron
that ejected with a finite kinetic energyEꢀ:
ꢥꢜ = ꢥꢦ − ꢥꢧ
(2)
where, Eꢨ is the energy of the incident photon, Eꢩ is the electronic binding energy [34,35].
However, not all the photons of the incident gammaray could interact with perovskite (Figure
5b). The PE interaction cross-section is inversely proportional to gamma photon energy and
Zꢄ
atomic number, can be estimated as τꢪꢫ
∝
ꢬ.ꢭ, where exponent n in the range of 4 to 5.
ꢮ
Eꢨ
It is to be noticed that the slightly enhanced shielding performance of Br-doped materials is
μ
mainly caused by the K-shell of Br. The shielding performance (large value of ( ꢊ ) and thin
ρ

HVL) at 100keV is better than at 60keV, this phenomenon is attributed to K-shell absorption
edge of Pb [36].
3.4 Stability
Fig. 6. Radiation stability: (a) intensity shielding efficiency of crystal, as grown and
after radiation (b) comparison of pulse height spectra of Pu-238 radiation source after
shielded by as-grown and after radiation MAPbCl3 SCs crystals. The radiation gamma
ray is from Co-60 source, after exposure for 8h with the dose rate of 5520Gy.
Radiation stability is another concerned problem for applications, therefore, we have
evaluated the shielding stability of perovskite crystals under gamma ray. The crystals
were loaded into the radiation room in Co-60 radiation center at Nanjing University of
Aeronautics and Astronautics in the air at room temperature. The total exposure
radiation dose rate is up to 5520Gy after 8h exposure. No significant degradation of
shielding performance has been observed as shown in Figure 6a, b. The weak
shielding efficiency degradation is mainly attributed to ion immigration under the
photon irradiation, which is also demonstrated in previous literature [37,38].
4. Conclusions
High-quality MAPbBrxCl3-x single crystals have been obtained by using a solution
growth method at low temperature. The X(γ) photons radiation shielding properties

(mass attenuation coefficients, effective atomic numbers, half value layer) of
MAPbBrxCl3-x SCs have been systematically investigated, and the radiation
performances can be enhanced by the Br concentration. The perovskite crystals
exhibited ultra-stability under a high dose rate of gamma ray irradiation. In addition,
the crystals exhibit high transparency in the visible range with tunable cut-off edge
and refractive index. These results indicate that the MAPbBrxCl3-x SCs is optimal to
provide radiation shielding that requires a visual clarity and radiation shielding
applications, especially for medical treatment, imaging, diagnostic and industrial
workplace.
Acknowledgements
This work was supported by the National Natural Science Foundation of China
(11705090, 11875166, 11435010).
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1. The shielding performance for gamma ray (59keV) is more than 10 times higher
than that of polymer composites.
2. The organic–inorganic perovskites exhibit high radiation stability under 60Co
gamma ray irradiation with dose rate up to 5520Gy after 8h exposure in air at room
temperature.
3. The shielding performances and optical properties can be slightly tuned by halide
Br doping concentration