Simple synthesis-controlled fabrication of thallium cadmium iodide nanostructures via a novel route and photocatalytic investigation in degradation of toxic dyes

Article abstract of DOI:10.1016/j.ica.2016.10.015

The present work focused on the synthesis and characterization of TlCdI₃nanostructures through a new mechanical mixture of the reactants method for the first time. In this work, thallium nitrate, cadmium nitrate and lithium iodide were chosen as starting reagents. The preparation of CdI₂and TlI for synthesis of TlCdI₃were performed at ambient condition. The morphology, phase structure, and phase purity of TlCdI₃can be controlled by the TlI:CdI₂ratio and also adjusting type of surfactant. In our experimental conditions, the ideal ratios between TlI:CdI₂was 1:1, Also the ideal surfactant was SDS. The nanostructures were characterized by using XRD, SEM, TEM, EDS and FT-IR. The photocatalytic activity of the synthesized products has been compared in the photodegradation activity of methyl orange (MO) and methylene blue (MB).

Full text of DOI:10.1016/j.ica.2016.10.015

Accepted Manuscript
Research paper
Simple synthesis-controlled fabrication of thallium cadmium iodide nanostruc-
tures via a novel route and photocatalytic investigation in degradation of toxic
dyes
Mojgan Ghanbari, Fatemeh Ansari, Masoud Salavati-Niasari
PII:
S0020-1693(16)30669-7
http://dx.doi.org/10.1016/j.ica.2016.10.015
ICA 17308
DOI:
Reference:
To appear in:
Inorganica Chimica Acta
Received Date:
Revised Date:
Accepted Date:
9 August 2016
5 October 2016
9 October 2016
Please cite this article as: M. Ghanbari, F. Ansari, M. Salavati-Niasari, Simple synthesis-controlled fabrication of
thallium cadmium iodide nanostructures via a novel route and photocatalytic investigation in degradation of toxic
dyes, Inorganica Chimica Acta (2016), doi: http://dx.doi.org/10.1016/j.ica.2016.10.015
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Simple synthesis-controlled fabrication of thallium cadmium iodide nanostructures via a
novel route and photocatalytic investigation in degradation of toxic dyes
a
b
c*
Mojgan Ghanbari , Fatemeh Ansari , Masoud Salavati-Niasari
a
Institute of Nano Science and Nano Technology, University of Kashan, Kashan, P. O. Box. 87317-51167, I. R.
Iran
b
Faculty of Science, Islamic Azad University, Science and Research Branch, Tehran
*
Corresponding author. Tel.: +98 31 55912383; Fax: +98 31 55913201
E-mail address: salavati@kashanu.ac.ir (Prof. Masoud Salavati-Niasari)
Abstract The present work focused on the synthesis and characterization of TlCdI
new mechanical mixture of the reactants method for the first time. In this work, thallium nitrate, cadmium nitrate
and lithium iodide were chosen as starting reagents. The preparation of CdI and TlI for synthesis of TlCdI were
performed at ambient condition. The morphology, phase structure, and phase purity of TlCdI can be controlled
by the TlI:CdI ratio and also adjusting type of surfactant. In our experimental conditions, the ideal ratios between
TlI:CdI was 1:1, Also the ideal surfactant was SDS. The nanostructures were characterized by using XRD, SEM,
3
nanostructures through a
2
3
3
2
2
TEM, EDS and FT-IR. The photocatalytic activity of the synthesized products has been compared in the
photodegradation activity of methyl orange (MO) and methylen blue (MB).
Keywords: Nanostructure; TlCdI
. Introduction
3
; Surfactant; Photocatalytic; Optical property; Electron microscopy.
1
1

In recent years Metal halide perovskites are currently under intense investigations because of their potential
application in photoelectronic devises [1-4] and as light emitting diodes, photodetectors, and lasers [5-8]. The
perovskite structure is a highly versatile and widespread mineral form, of great importance in nature and
technology. They were first suggested by the Russian mineralogist Count Lev Aleksevich von Perovski, who
discovered the naturally occurring mineral calcium titanate (CaTiO ) [9]. The stability of pervoskite structure is
3
necessary for this the sum of positive and negative charges be equal to the crystal lattice charge becomes zero. In
halide Perovskite the sum of halide ions charge is equal to -3, as a result the sum of cations charge must be equal
to +3 [9, 10]. Many halide perovskites with the general formula AMX
Br, I) are built face-shared, corner-shared,edge-shared orpartlyface-partly corner-shared form of [MX
octahedrons [11-14] of special interest are the group 14 iodometalates, since they can adopt perovskitic structures
that are amenable to compositional variation. In the perovskite formula, AMX , when the A-site in structure, is
occupied by a small monovalent cation, such as Rb, Cs, K is obtained a three-dimensional (3D) framework [15,
3
(A = Cs, Rb;Tl; M = Cd, Mg, Ni; X = Cl,
]
6 4
3
1
2
6]. If a larger cation is used instead two-dimensional (2D) layered [17, 18] or one-dimensional (1D) chain [19,
0]. Materials are obtained with formulas AMI , A MI and A MI which still retain their perovskite [21, 22]. The
3
2
4
3
structure of these compounds is extremely dependent on the stoichiometry of the final material and the metal-
halide linkages [23].
Nanomaterials have been synthesized by hydrothermal [24], reverse-micelle [25], chemical co-precipitation [26],
auto-combustion sol-gel technique [27-30], glass-crystallization [31], and salt melt methods [32]. But
precipitation is an effective method for the synthesis because this technique provides a simple and appropriate
approach for preparation of nanometerials and has many advantages: low cost, easy component adjustment, and
high homogeneity of the obtained nanomaterials [33]. In this work the nanostructures of TlCdI were synthesized
3
by simple mechanical mixture of the reactants method in ambient condition, Accordingly, neither high-
2

temperature, complex chemical reactions nor high-vacuum deposition processes are required, contrary to most
conventional methods that have been used for synthesis these materials. Finally products were characterized by
XRD, SEM, TEM, EDS, FT-IR, DRS and UV-Vis
2
. Experimental
2
.1. Materials and experiments
All the chemicals used in our experiments were of analytical grade, were purchased from Merck and used
as received without further purification. XRD patterns were collected from a diffractometer of Philips Company
with X'PertPro monochromatized Cu Kα radiation (λ = 1.54 Å). GC-2550TG (Teif Gostar Faraz Company, Iran)
were used for all chemical analyses. FE-SEM images were obtained on MIRA3 FEG-SEM.. The EDS analysis
was studied by XL30, Philips microscope.
2
.2. Synthetic of TlCdI
3
TlCdI
and LiI were dissolved in separate Beakers in distilled water. The preparation of CdI
point Cd(NO was used as Cd source and stoichiometry amount of Cd(NO and LiI were dissolved in separate
Beakers in distilled water to form a clear solution. Following TlI and CdI
3
has been synthesized from precorsur TlI and CdI
2
. For synthesis of TlI stoichiometry amount of TlNO
3
2
is similar to TlI for this
3
)
2
)
3 2
2
were mixed together with a curtained
°
ratio and grinned in mortar for 2h and the result powder were dried in oven at 70 C. the effect of different
parameters was investigated on the morphology and phase purity of the products. Table 1 lists the reaction
conditions for the synthesis of TlCdI3. Scheme 1 shows a schematic diagram of the formation process of the
TlCdI
3
nanostructures.
2
.3. Photocatalytic experiment
3

The photocatalytic activities of the samples are determined by the degradation of aqueous methyl orange (MO)
and methylene blue (MB) under UV light in presence of TlCdI (0.005ꢀg/L) is first inserted to a reactor that
3
included about (0.1ꢀmM) of aqueous MO and MB. Then the suspension is transferred into a self-designed glass
reactor, and stirred in darkness to attain the adsorption equilibrium. In the investigation of photodegradation using
UV light, a 125 W high-pressure mercury lamp with a water cooling cylindrical jacket is utilized. The
concentration of MO and MB is checked on the basis of its UV-visible absorption.
3
. Results and discussion
XRD analysis, which is the most useful technique for identification of crystalline structure, was employed to
investigate the prepared samples. The XRD patterns for the samples no: 1, 2, 3 and 4 are shown in Fig. 1a-d,
respectively. When the ratio of TlI/CdI is 1:1 and 1:0.75 (sample no. 1 and 4), the products have the peaks
corresponding to pure TlCdI (JCPDS NO 70-2182) as shown in XRD patterns in Fig. 1a. Changing of the ratio of
TlI/ CdI from 1:1 to 2:1 (sample no. 2) and 1:2 (sample no. 3), a mixture of TlCdI and Tl CdI (JCPDS NO 79-
303) in Fig. 1b and TlCdI and CdI (JCPDS NO 33-0239) in Fig. 1c are obtained respectively.
In the following the effect of surfactants (NaHSal, CTAB, SDS, Triplex and PVA) on the purity of the products
were investigated. Fig. 2a-f shows the XRD patterns of products (sample no. 5, 6, 7, 8 and 9) obtained in the
2
3
,
2
3
4
6
1
,
3
2
presence of different surfactants. This figure clearly shows the formation of TlCdI
SDS.
3
only occur in the presence of
The morphology of the samples was investigated by SEM images. Fig. 3 shows the SEM images of samples
achieved with different ratios of TlI/CdI involving (a) 1:1, (b) 2:1, (c) 1:2 and 1:0.75 (d). It can be seen that the
bulk structures are formed when the molar ratio of TlI/CdI is 2:1 and 1:0.75 (sample no. 2 and 4). The sphere-
2
2
like nanostructures in sample no. 1 and 3 are aggregated as shown in Fig. 3 c and d, whereas in the sample no. 1
4

these structures are apart from one another (Fig. 3 c). Thus, in our experimental conditions, the ideal ratio
between TlI/CdI is 1:1. In continuation, the effect of the surfactant on the morphology of the products was
investigated, whereas the molar ratio between TlI and CdI was selected to be 1:1. Fig. 4 shows the SEM images
of the TlCdI obtained in the presence of different surfactants. It can be observed that agglomerated
nanostructures with different shapes and sizes have been formed in the presence of NaHSal (Fig. 3a), CTAB (Fig.
b), SDS (Fig. 3c) PVA (Fig. 3d) and Triplex (Fig. 3f). In the presence of NaHSal, CTAB, SDS, Triplex and
2
2
3
3
PVA The morphology of product are not suitable and not regular. The sample obtained in the presence SDS has
spherical morphology as shown in Fig. 4 c. The nanoparticles in this figure have more even distribution than other
samples. Thus, in our experimental conditions, the ideal surfactant is SDS. Typical histograms of the particle
diameters for the samples Nos. 1, 2, 3, 5,6, 7, 8 and 9 are seen in Fig. 5a–h, respectively.
The detailed morphology and particle size of the as-obtained TlCdI nanostructures (sample no. 1) was
3
investigated by transmission electron microscopy (TEM). The TEM image (Fig. 5) demonstrates that thallium
cadmium iodide nanoparticles with diameter from 10 to 50 nm have sphere-like shape.
EDS analysis measurement was employed to investigate the chemical composition and purity of as-synthesized
TlCdI nanostructures. Fig. 6 shows the EDS spectrum of the sample no 1. This figure shows only the presence of
3
Tl, Cd and I elements in the product.
The optical absorption spectrum of TlCdI nanoparticles represents in Fig. 7a The DRS spectrum was used to
3
further access their quality and electronic structure information. It demonstrates a major absorption peaks about
0 nm and different low intensity absorption peaks in 100-300 nm. The others absorption bands have been
attributed to the impurities or vacancies. The optical band gap of TlCdI has been evaluated using the optical
8
3
density (OD) vs. energy (E) plot (Fig. 7a). The value of band gap energy for this nanoparticle is ~ 2.9 eV. To
5

prove the photocatalytic activity of samples for the degradation pollutants, the photocatalytic degradation of MO
and MB experiments were performed as a model reaction under UV light irradiation. The percentage of
degradation %D was determined as follows:
Where A
catalytic activity of TlCdI
illustrates the UV-Vis spectra of aqueous solution of MO and MB (0.1ꢀmM) in presence of TlCdI
different irradiation times. When TlCdI nanopowder is irradiated by light with energy greater than or equal to
0
and A are the absorbencies of the liquid sample before and after degradation, respectively. The photo-
powder was investigated by degradation of MO and MB as organic pollution. Fig. 7b
(0.005ꢀg/L) at
3
3
3
band-gap, an electron in the valence band could be excited to the conduction band, as a result a hole generated in
the valance band. These electron-hole pair that generated by UV-light can also recombines or interacts
independently with other molecules in aqueous solution. The holes in the valence band could be reacted with
water on the surface of TlCdI
3
or hydroxide ions and produced extremely reactive hydroxyl radicals (˙OH)
−
whereas electrons could accept oxygen by adsorption and shaped superoxide radical anion (O
2
). This radical may
form organic peroxides or H
2
O
2
in presence of organic adsorbent. The hydroxyl radical is a very strong oxidizing
agent and aggress the dye molecule to provide the oxidized product. The reactions could be summarized in
following reactions [34-35].
+
-
TlCdI + hν → h + e
3
6

4
. Conclusions
In this work the nanostructures of TlCdI were synthesized by simple mechanical mixture of the reactants
3
method in ambient condition, Accordingly, neither high-temperature, complex chemical reactions nor high-
vacuum deposition processes are required, contrary to most conventional methods that have been used for
sybthesise these materials. The effect of molar ratio of TlI:CdI
and crystallinity of products were investigated. we could obtain the nanostructures with desired morphology. To
the best of our knowledge, it is the first time that nanostructures of TlCdI are synthesized in ambient condition
2
and different surfactants on morphology, purity
3
also it is the first time that precipitation route are used for the synthesis of these materials. The method is proved
to be a new, simple, efficient and quick way.
Acknowledgment
Authors are grateful to the council of Iran National Science Foundation and University of Kashan for supporting
this work by Grant No (159271/5746).
7

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12

Figure captions
Fig. 1. XRD patterns of samples prepared: (a) with ratio of 1:1 of TlI:CdI
2
(sample no. 1) , (b) ratio of 1:2
(sample no. 4).
TlI:CdI
2
(sample no. 2), (c) ratio of 2:1 of TlI:CdI
2
(sample no. 3), (d) ratio of 1:0.75 of TlI:CdI
2
Fig. 2. XRD patterns of samples prepared with 1:1 ratio of TlI:CdI
2
, in the presence of: (a) NaHsal (sample no. 5),
(
b) CTAB (sample no. 6) , (c) SDS (sample no. 7) , (d) triplex (sample no. 8) and (f) PVA (sample no. 9).
Fig. 3. SEM images of TlCdI
3
nanostructures prepared with different ratios of TlI:CdI : (a) with ratio of 1:1
2
(
sample no. 1) , (b) ratio of 1:2 (sample no. 2) , (c) ratio of 2:1 (sample no. 3) , (d) ratio of 1:0.75 (sample no. 4).
Fig. 4. SEM images of TlCdI
3
prepared with 1:1 ratio of TlI:CdI , in the presence of: (a) NaHsal (sample no. 5),
2
(
b) CTAB (sample no. 6) , (c) SDS (sample no. 7) , (d) triplex (sample no. 8) and (f) PVA (sample no. 9).
Fig. 5. Particle size distribution of samples Nos. (a) 1, (b) 2, (c) 3, (d) 5, (e) 6, (f) 7, (g) 8 and (h) 9.
Fig. 6. TEM images of TlCdI
3
nanostructures prepared with ratio of 1:1 of TlI:CdI (sample no. 1).
2
Fig. 7. EDS patterns of TlCdI
3
nanostructures (sample no. 1).
2
Fig. 8. (a) DRS spectrum (b) optical density (αhν) vs. energy (c) UV-Vis spectra of photodegradation of MO and
MB with TlCdI as a function of time.
3
Table 1. The reaction conditions of TlCdI
3
synthesized in this work.
Scheme 1. shows a schematic diagram of the formation process of the TlCdI
3
nanostructures.
13

Fig 1.
14

Fig 2.
15

Fig 3.
16

Fig 4.
17

Fig. 5
18

Fig 6.
19

Fig. 7.
20

Fig. 8.
21

Table 1.
Sample. no
Precursors Ratio
TlI + CdI
Surfactant
1
2
3
4
5
6
7
8
9
2
-
TlI + 2CdI
2TlI + CdI
2
2
-
-
TlI + 0.75CdI
2
-
TlI + CdI
TlI + CdI
TlI + CdI
TlI + CdI
TlI + CdI
2
2
2
2
2
NaHSal
CTAB
SDS
Triplex
PVA
22

Scheme 1.
23

The present work focused on the synthesis and characterization of TlCdI nanostructures through a new
3
mechanical mixture of the reactants method for the first time. The photocatalytic activity of the synthesized
products has been compared in the photodegradation activity.
25

ꢀ
ꢀ
ꢀ
TlCdI
Synthesise of TlCdI
Optimum condition for preparation TlCdI
The nanostructures were characterized by using XRD, SEM, TEM, EDS and FT-IR.
The photocatalytic activity of the TlCdI has been compared in the photodegradation activity.
3
nanoparticles have been synthesized by precipitation method.
nanostructures in ambient condition.
nanostructures investigated.
3
3
ꢀ
ꢀ
3
26