Synthesis, Raman spectroscopy and dielectric properties of Ag:Mn co-doped nanostructured PbI2 for solid state radiation detectors

Article abstract of DOI:10.1016/j.molstruc.2017.03.016

Microwave-assisted synthesis of pure and Ag: Mn co-doped PbI₂ nanostructures have been reported for the first time. The structural and vibrational confirmations were carried out by X-ray diffraction and FT-Raman spectroscopic analysis. Furtherm

Full text of DOI:10.1016/j.molstruc.2017.03.016

Journal of Molecular Structure 1138 (2017) 215e221
Contents lists available at ScienceDirect
Journal of Molecular Structure
journal homepage: http://www.elsevier.com/locate/molstruc
Synthesis, Raman spectroscopy and dielectric properties of Ag:Mn co-
doped nanostructured PbI for solid state radiation detectors
2
a, b, *
, M.M. Abutalib c
I.S. Yahia
a
Advanced Functional Materials & Optoelectronic Laboratory (AFMOL), Department of Physics, Faculty of Science, King Khalid University, P.O. Box 9004,
Abha, Saudi Arabia
b
Nanoscience Laboratory for Environmental and Bio-medical Applications (NLEBA), Semiconductor Lab., Department of Physics, Faculty of Education, Ain
Shams University, Roxy, 11757 Cairo, Egypt
c
Physics Department, Faculty of Science-AL Faisaliah Campus, King Abdulaziz University, Jeddah, Saudi Arabia
a r t i c l e i n f o
a b s t r a c t
Article history:
Received 13 January 2017
Received in revised form
Microwave-assisted synthesis of pure and Ag: Mn co-doped PbI2 nanostructures have been reported for
the first time. The structural and vibrational confirmations were carried out by X-ray diffraction and FT-
Raman spectroscopic analysis. Furthermore, the EDX analysis confirms the presence of Ag and Mn in PbI
2
1
March 2017
nanostructures. No extra phase due to impurity in the synthesized nanostructures was observed. The
nanosheets like morphology were confirmed by SEM study for all the synthesized products. The average
thicknesses of the prepared nanosheets are found to be in the range of ~30 nme50 nm. The dielectric
Accepted 3 March 2017
2
constant is found to be enriched by Mn and Ag: Mn co-doping in PbI compared to bulk value. The
organized nanostructure with enhanced physical properties warrants the applications in optoelectronic
devices and nanoscale radiation detectors.
Keywords:
Lead iodide
Semiconductor
X-ray diffraction
SEM
© 2017 Elsevier B.V. All rights reserved.
Optical properties
Gamma radiation detector
1. Introduction
diverse methods and found good variation in the properties
compare to bulk [12e18]. Recently, the synthesis of pure and doped
Nanostructured materials of semiconductors are of great
importance for optoelectronic industries. The nanomaterials with
organized morphology are one of the amazing areas of research due
to their wide range of use in fabrication of optoelectronic devices
2
nanostructures of PbI with enhanced physical properties using
hydrothermal and microwave irradiation techniques are reported
by our group [17e19]. Due to the astonishing application of the title
materials, it seems to be necessary and justified to prepare the
nanostructures using suitable dopants and techniques with
enhanced properties from an application point of view.
[
1e3]. It is well documented in the literature that the wide band
gap semiconductors are ideal options for nanostructured materials
4e7].
Lead iodide is an appropriate wide band gap semiconductor
[
Hence, the authors have decided to prepare the pure, doped and
co-doped nanostructures of PbI with organized morphology using a
2
which has several applications as in active matrix flat-panel im-
agers (AMFPIs), applied in X-ray digital radiography detector,
mammography, photoconductors, photodetectors, biological la-
beling and diagnostic, LEDs etc. [8e11]. As per the available liter-
ature, numerous reports are documented on the nanostructure
microwave-assisted method that provides volumetric and homo-
geneous heating to the materials [19e21]. The synthesized nano-
structures are studied by powder X-ray diffraction, FT-Raman,
Energy-dispersive X-ray spectroscopy/scanning electron microscopy
(EDX/SEM), dielectric and gamma radiation measurement tech-
niques and analysis of the obtained data is done and discussed here.
synthesis and characterizations of pure and doped PbI
2
using
2. Experimental details
*
Corresponding author. Permanent address: Nanoscience Laboratory for Envi-
ronmental and Bio-medical Applications (NLEBA), Semiconductor Lab., Department
of Physics, Faculty of Education, Ain Shams University, Roxy, 11757 Cairo, Egypt.
E-mail addresses: dr_isyahia@yahoo.com, isyahia@gmail.com, ihussein@kku.
edu.sa (I.S. Yahia).
2
.1. Materials
In the current work, Lead (II) acetate trihydrate, sodium iodide,
http://dx.doi.org/10.1016/j.molstruc.2017.03.016
0
022-2860/© 2017 Elsevier B.V. All rights reserved.

216
I.S. Yahia, M.M. Abutalib / Journal of Molecular Structure 1138 (2017) 215e221
Poly(vinyl alcohol) (PVA), Cetyltrimethylammonium bromide
CTAB), Silver nitrate and manganese (II) nitrate hydrate were
purchased from Sigma-Aldrich and were used without any further
10
20
30
40
50
60
70
80
(
7.5% Ag doped Mn:PbI2
purification.
2.2. Synthesis of Ag co-doped nanostructured Mn:PbI
2
5% Ag doped Mn:PbI2
For the synthesis of Silver and Manganese (Ag:Mn) co-doped
2
nanostructures, the following procedure was done: (1) for
PbI
pure PbI
2
: the Calculated amount of 1 M (lead acetate trihydrate)
ꢀ
was taken and dispersed in double distilled (DD) water at 80 C by
continuous stirring. In the prepared solution, 50 ml of PVA (45 g/l)
and 50 ml of CTAB (15 g/l) were added slowly one by one. (2) The
solution of NaI (2 M) was prepared in 100 ml DD water which was
dropwise added to the above-prepared solution by continuous
stirring at the same temperature and instantly the yellow precipi-
tate was produced. The yellow color confirms the formation of lead
iodide. The same procedure was applied to prepare the Ag:Mn:PbI2
with different concentrations of Mn and Ag. For Mn doping, 10 wt%
of Manganese Nitrate hydrate has been taken in another beaker and
dissolved in 50 ml DD water. This prepared solution was slowly
added to the prepared solutions to have Mn doping. Furthermore,
for Ag doping, we have prepared the solution of silver nitrate of
different concentrations from 1 to 7 wt % in 50 ml DD water and
added to the above prepared five sets to have Mn:Ag co-doping in
2.5% Ag doped Mn:PbI2
1% Ag doped Mn:PbI2
1
0 % Mn:PbI2
pure PbI2
70
2
PbI matrix. Once all the six sets i.e. one pure and 5 doped solutions
are ready, we subjected them to microwave radiation for a constant
time (i.e. 15 min) using the modified domestic LG-microwave
10
20
30
40
50
60
80
(
7
Model No. MS5246VR/00) of frequency 2.54 GHz and operated at
00 W power. All the solutions were naturally cooled down to the
o
2Theta
room temperature and taken out from the microwave. The finally
prepared nanostructured lead iodide solutions were filtered and
washed several times by DD water as well as ethanol to have high
Fig. 1. Powder X-ray diffraction patterns of synthesized nanostructures PbI
with Ag:Mn.
2
co-doped
purity nanostructures. The filtered nanostructures were kept inside
the oven at 80 C for about 24 h to remove any moisture and sub-
jected to different characterizations.
ꢀ
of X-ray peaks is very high which confirms that the prepared
nanostructures are of good crystalline nature. From the analysis of
the recorded XRD data of all the specimens using attached software
to the XRD device, the single phase was confirmed and unit cell
parameters were determined. The refined cell parameters are
presented in Table 1 and found to be correlated well with earlier
data JCPDS No. 07-0235. From the data, the dominant hexagonal
phase of 2H-polytype of PbI was confirmed for all the prepared
2
nanostructures. The variation in the main peaks position with hkl
planes are presented in Table 1 which clearly shows that the doping
2.3. Characterization techniques
For structural confirmation and lattice parameter calculations,
all the prepared nanostructures were subjected to powder X-ray
diffraction measurement using Shimadzu LabX-XRD-6000 X-ray
diffractometer with CuK
a
(
l
¼ 1.5406 Å) radiation and the matching
of the recorded data was done using the attached Shimadzu soft-
ware with the pdf-2 library. The surface topography of all the
nanostructures was recorded using scanning electron microscope
(
JSM-6360) operated at 20 kV. For vibrational analysis, the pre-
Table 1
pared nanostructures were subjected to FT-Raman spectroscopy
measurements using THERMO FISHER SCIENTIFIC, DXR FT-Raman
spectrometer using the 532 nm laser excitation source operated
The change of the preferred ordination with doping of synthesized nanostructured
of PbI
Sample name
Pure-PbI
2
co-doped with Ag:Mn.
ꢀ
2theta ( )
Planes (hkl)
Intensity, (a.u.)
ꢁ
1
at 0.2 mW power in the wavenumber range of 20e500 cm , at
2
12.5692
001
002
101
001
002
101
001
002
101
001
002
101
001
002
001
002
101
100
90
12
88
11
100
81
6
ꢁ1
estimated resolution 5.1e8.3 cm . A well computer-controlled
Keithley 4200-SCS semiconductor characterization system was
used for dielectric and ac conductivity measurements. Gamma
linear absorption coefficient was determined using a gamma ray
source (Am-241) of energy (59.5 KeV) for the duration about
25.88
26.28
10% Mn-doped PbI
2
12.7144
2
2
5.54
5.9972
1
2
% Ag-doped Mn:PbI
2
12.792
100 s at room temperature.
2
2
5.42
6.0472
100
100
7
60
37
18
29
32
20
.5% Ag-doped Mn:PbI
2
12.9184
3
. Results and discussion
2
2
5.72
6.2021
2
3.1. Structural analysis of synthesized nanostructured PbI co-
5
7
% Ag-doped Mn:PbI
2
12.7572
26.0208
12.6346
doped with Ag:Mn
.5% Ag-doped Mn:PbI
2
2
2
5.9
6.02
Fig. 1 shows the recorded XRD patterns of all the prepared
nanostructures. It can be observed from the figure that the intensity

I.S. Yahia, M.M. Abutalib / Journal of Molecular Structure 1138 (2017) 215e221
217
Table 2
The calculated mean values of grain size, dislocation density and strain of synthe-
b
cos
4
q
ε ¼
;
(3)
sized nanostructures PbI
2
co-doped with Ag:Mn.
ꢁ2
ꢁ4
)
Mean values
D, (nm)
d
, (lin. nmꢁ2)
ε, (lin
m
where the symbols are having their usual meanings. The calculated
values of these parameters are tabulated in Table 2. From the
tabulated data it is clear that the value of D is increased by doping
Pure-PbI
2
34.710
31.355
34.639
55.555
54.320
44.474
1.40E-03
1.36E-03
1.21E-03
4.66E-04
8.78E-04
1.20E-03
1.22E-03
1.23E-03
1.08E-03
6.96E-04
8.84E-04
1.11E-03
1
1
2
5
7
0% Mn-doped PbI
% Ag-doped Mn:PbI
.5% Ag-doped Mn:PbI
% Ag-doped Mn:PbI
.5% Ag-doped Mn:PbI
2
2
and d and ε are found to be reduced.
2
2
2
3.2. Analysis of EDX/SEM of synthesized nanostructured PbI
2
co-
doped with Ag:Mn
The recorded EDX spectra for pure and doped nanostructures
2
are shown in Fig. 2(aef). Initially, the Mn doping was
PbI
confirmed as shown in Fig. 2(b). Further, the Mn and Ag both were
confirmed as shown in Fig. 2(cef). The doping was also confirmed
by EDX in PbI
aimed doping has been successfully achieved in lead iodide nano-
structures. The SEM micrographs for pure and doped PbI nano-
2
previously [18,19]. So it can be concluded that the
2
structures are shown in Fig. 3(aef). From this figure, it is clear that
the prepared nanostructures for pure as well as doped are nano-
sheets of thicknesses in the range of ~30 nme50 nm. No major
change was observed due to doping in the morphology of the
nanostructures; however, the density of nanosheets has been
increased with doping. A similar type of results was also reported
3þ
for Gd
concluded that the Mn and Ag doping is not having a major effect
on the morphology of PbI except increasing the d of nanosheets.
doped PbI
2
nanostructures recently [18]. It may be
2
However, the change in the thicknesses of the prepared nano-
structures is found to be varied with doping. All the nanosheets
have a very minute variation in the thicknesses throughout the
samples which confirm their homogeneity and found in agreement
to XRD parameters. It can be clearly seen in SEM image for 7.5% Ag-
2
doped Mn:PbI [Fig. 3(f)] that it contains a high density of nano-
sheets compare to others. This suggests that at this particular
concentration we can achieve high-density number of nanosheets
with almost homogeneous thickness at large scale.
3.3. Vibrational analysis of synthesized nanostructured of PbI
2
co-
doped with Ag:Mn
2
Fig. 2. (aef). EDX spectra of synthesized nanostructured PbI (a) pure, (b) 10% Mn, (c)
1% Ag:Mn, (d) 2.5% Ag:Mn, (e) 5% Ag:Mn and (f) 7.5% Ag:Mn.
The recorded FT-Raman spectra of all the prepared nano-
structures are shown in Fig. 4. The key vibration bands are observed
at ~33.83, 71.44, 95.54, 108.08, 165.93, 216.08 cm (pure), 33.84,
ꢁ
1
2
is taking place in PbI . The presence of Ag was also investigated
ꢁ
1
very deeply by comparing the JCPDS card data of Ag and AgI and
found that at higher concentration (i.e. 5% and 7.5% Ag), the sec-
ondary phase as cubic AgI was observed. The peaks of AgI were
7
4
1.44, 94.58, 108.08, 165.93, 215.11 cm
(10% Mn:PbI
2
), 33.84,
ꢁ
1
9.27vw, 70.48, 94.58, 108.08, 164.97, 214.15 cm (1% Ag co-doped
ꢁ1
Mn:PbI
2
), 33.83, 49.27, 69.51, 94.58, 108.08, 164.97, 214.17 cm
), 33.84, 71.44, 94.58, 109.05, 165.94,
14.15 cm (5% Ag co-doped Mn:PbI ), 33.84, 51.20, 68.55, 95.58,
(7.5% Ag co-doped Mn:PbI ) nano-
structures readied by microwave-assisted technique. These vibra-
ꢀ
ꢀ
ꢀ
found at angle 23.67 (111), 46.345 (311) and 62.59 (331) which
are well matched with JCPDS No. 9-0399. Also at higher concen-
(2.5% Ag co-doped Mn:PbI
2
ꢁ1
2
2
ꢁ1
tration of Ag-doped Mn:PbI
2
, the free iodine peak was also
108.08, 165.94, 213.18 cm
2
ꢀ
observed at 15.2 (110), which is slightly at a lower angle than the
pure I (JCPDS No. 35-1002). Such peaks due to free iodine can be
expected in the prepared system due to the high reactivity of Ag
with iodine as well as Pb with iodine. Furthermore, the crystallite
1
1
2
1
1
tion bands are attributed to E
respectively [12,23,24].
The vibration band at low wavenumber i.e. ~34 cm can be
assigned to breathing motion of PbI layers [17,18,25]. The observed
bands for all the prepared nanostructures are found to be compa-
rable with the previously reported bands for PbI nanostructures
17,18,26]. All the vibrational modes are found to be shifted in
2 1 1 u 2 1
, A , A , 2E , A2u, 2E and 2E ,
ꢁ
1
size (D), dislocation density (
d) and lattice strain (ε) were evaluated
2
for all the nanostructures using the Scherer's formula [22]:
2
[
D ¼ b0
:9
cos
l
;
(1)
(2)
ꢁ1
comparison of bulk values 74, 97, 112, 151, 172, 214 and 226 cm
26]. These observed bands confirm the formation of 2H Polytypes
of PbI and found in correlation with structural results in the pre-
sent work as well as with previous reports on pure and doped PbI
q
[
2
d
¼
D
1 ;
2
nanostructures [17,25]. The shift in bands is may be due to extra
relaxed binding in nanosheets due to their larger surface to volume
ratio. It can be seen in figure that the Raman intensity of peaks is
and

218
I.S. Yahia, M.M. Abutalib / Journal of Molecular Structure 1138 (2017) 215e221
(a)
(b)
(c)
(d)
(e)
(f)
2
Fig. 3. (aef). SEM micrographs of (a) pure, (b) 10% Mn, (c) 1% Ag:Mn, (d) 2.5% Ag:Mn, (e) 5% Ag:Mn and (f) 7.5% Ag:Mn co-doped PbI nanostructures.
20000
18000
16000
14000
12000
10000
Pure
0% Mn
1.0% Ag doped Mn:PbI2
1
2
.5% Ag doped Mn:PbI2
.0% Ag doped Mn:PbI2
5
7.5% Ag doped Mn:PbI2
8000
6000
4000
2000
0
500
400
300
200
100
-
1
Raman shift (cm )
Fig. 4. FT-Raman spectra of synthesized nanostructured of PbI
2
co-doped with Mn:Ag.

I.S. Yahia, M.M. Abutalib / Journal of Molecular Structure 1138 (2017) 215e221
219
enriched due to doping at some concentrations (10% Mn, 1%, and
.5% Ag co-doped Mn:PbI ), however at some concentrations (5%
and 7.5% Ag co-doped Mn:PbI ), it was found to be reduced as well.
Ag:Mn:PbI
pure PbI . The calculated ε1 values for the synthesized nano-
structures are found to be higher than the previously reported value
for bulk single crystals of PbI [33,34]. However, the values observed
2
nanostructures is found to be enriched compared to
2
2
2
2
2
in the current work are lower than the previously reported work by
our group on nanostructured pure and doped lead iodide [17,18].
The reason behind low values is may be due to shape, orientation,
3
.4. Dielectric and ac electrical conductivity analysis of synthesized
2
nanostructured PbI co-doped with Ag:Mn
size and structural parameters. The dielectric loss (ε ) also depends
2
It is well known that the dielectric properties are changed due to
change in the size of particles, shapes, and boundaries [27] and the
nanostructure with modified dielectric properties can be applied in
optoelectronic devices like capacitors, memories, and filters. Hence,
we have measured the capacitance (C), impedance (Z) and loss
on the frequency [Fig. 5(b)] in the same way as dielectric constant
and its low value confirm the less defects nanostructures.
Furthermore, the ac electrical conductivity
computed by well-known relation:
ðsac:tot:Þ was
tangent (tan
Using the measured C, Z and tan
d
) in the high-frequency range from 3 kHz to 10 MHz.
l
s
ac:tot:
¼
;
(4)
d
data, dielectric constant and loss
Z ꢂ A
Cꢂ l
was calculated using the following relations: ε ¼
and
1
0
ε ꢂA
To know the conductivity mechanism the Jonscher's law was
used:
ε
¼ tan ꢂ ε ; respectively. Fig. 5(a&b) show the dielectric con-
d
2
1
stant (ε ), dielectric loss (ε ), plots with the applied frequency. The
1
2
value of dielectric constant is found to be almost stable in the tested
range which reliant on the actuality that the electric field and dipole
does not pursue the alternating field [28e32]. The ε1 values for
s
s
ac:tot:
¼
s
þ B
u
;
(5)
dc
1
3
Pure PbI2
(a)
(b)
Pure PbI2
0 % Mn-doped PbI2
Ag-doped Mn:PbI2
.5 % Ag-doped Mn:PbI2
Ag-doped Mn:PbI2
7
10 % Mn-doped PbI2
1
1 %
.5 % Ag-doped Mn:PbI2
5 % Ag-doped Mn:PbI2
7.5% Ag-doped Mn:PbI2
Ag-doped Mn:PbI2
1
%
12
6
5
4
3
2
1
0
2
2
5
%
7.5% Ag-doped Mn:PbI2
1
1
1
0
9
8
10
11
12
13
14
15
16
17
18
10
11
12
13
ln
14
15
16
17
18
lnω
, (ω
in Hz)
ω, (
ω
in Hz)
-
4
6
8
1
1
1
.060
.055
.050
(
c)
-
-
1.045
1
.040
.035
-10
-12
-14
1
Concentration of Ag
Pure PbI2
1
0 % Mn-doped PbI2
Ag-doped Mn:PbI2
.5 % Ag-doped Mn:PbI2
5 % Ag-doped Mn:PbI2
.5% Ag-doped Mn:PbI2
1
%
2
7
10
11
12
13
14
15
16
17
18
lnω, (ω in Hz)
2
Fig. 5. (aec). (a) Dielectric constant, (b) dielectric loss and (c) total ac electrical conductivity plots of synthesized nanostructured PbI co-doped with Mn:Ag.

220
I.S. Yahia, M.M. Abutalib / Journal of Molecular Structure 1138 (2017) 215e221
showed in Fig. 6(a). From which it can be concluded that the values
of are improved by doping and found to be analogous to other
reports [19,37,38]. The high value of
m
l
m
shows that the prepared
l
nanostructures can used for room temperature radiation detection.
The values of half value layer (HVL) ( x1=2), tenth value layer (TVL)
ðx
Þ, and mean free path (t) were also determined using the
1
=10
I ln 2 ln 10
ꢁ
m x
l
1
following relation [39,40]: ¼ e
2
; x
1
¼
, x
1
¼
and
m
. The obtained values of these are depict in Fig. 6(bed),
l
I
ο
2
m
l
10
m
l
t ¼ 1=
from figure it can be conclude that the value of x
1
is reduced with
2
doping and so the x1=10. Further, the value of MFP (t) also shows
same behavior as others. These results shows that the prepared
2
nanostructures of Ag:Mn:PbI are better contenders for radiation
detection at room temperature.
4. Conclusion
We have successfully synthesized the pure and Ag:Mn:PbI
with different concentrations) nanostructures by microwave-
2
(
assisted route for the first time. The single phase was confirmed
by X-ray diffraction and Raman analyses. The grain size is increased
however, dislocation density and lattice strain are found to be
reduced with doping. The morphology of the prepared nano-
structures are nanosheets and their thicknesses are found to be in
the range of 30e50 nm for all the synthesized samples confirmed
2
by SEM analysis. The density of nanosheets in the doped PbI was
found to be improved. The value of dielectric constant is increased
from 8.5 to 11 due to doping. The values of linear attenuation co-
efficient have been enriched in doped nanosheets which make it
more favorable for radiation detection to be used in medical health
applications. The enhanced properties warrant the application of
prepared nanostructures in electro-optic and radiation detection
devices.
Fig. 6. Linear attenuation coefficient, half value layer, tenth value layer and mean free
path for the prepared nanostructures.
where,
s
is the direct current conductivity, B is a constant and
u
is
angular frequency and s is an exponent of frequency. The calculated
ac:tot: with frequency is shown in Fig. 5(c). It can be observed from
figure that the value of ac:tot: is low and found to be reduced with
dc
Conflict of interest
s
s
The authors declare that there is no conflict of interest in the
current article.
reducing the frequency. Though, its value is higher for doped
nanostructures and it obeys the universal frequency power law. The
value of frequency exponent (s) is also calculated from the slope of
linear part of the curve ln
s
ac vs: ln
u
[see the inset of Fig. 5(c)]. Its
Acknowledgment
values are found vary from 1.044 to 1.073 for pure and doped
nanostructures and dependent of frequency. Generally its value is
observed in the range of 0.6 and 1 in ionic conducting materials [35]
though, its theoretical limit is ~1. As the value of s the prepared
nanostructures is ꢃ 1, which suggests that the hopping motion
involves a translational motion with sudden hopping.
This project was funded by the Deanship of Scientific Research
(DSR) at King Abdulaziz University, Jeddah under grant No. (G-471-
363-37). The authors, therefore, acknowledge with thanks for DSR
technical and finical support.
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3
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2
is a well-known radiation detector due to the
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)
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