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Influence of Mn2+ Incorporation on the Optical

Band Gap of ZnS Nanoparticles
G. G. Ramteke1*, A. S. Lanje2, D. M. Pimpalshende3
Department of Physics, Dr. Ambedkar College, Chandrapur, (M. S.), India1
Department of Electronics, Dr. Ambedkar College, Chandrapur, (M. S.), India2
Department of Physics, Dr. Ambedkar College, Chandrapur, (M. S.), India3
*
Corresponding author e-mail:ggramteke@gmail.com

Abstract: Undoped and Mn2+ doped ZnS semiconducting nanoparticles have enormously attracted due to
its stability and a wide variety of technological applications. It is an important semiconductor compound of
the II-VI group with an excellent physical, optical and electrical properties having wide band gap energy of
3.7 eV at room temperature. It has been extensively investigated due to its potential device applications
such as electroluminescent devices, data storage devices, efficient photo catalyst, quantum dot laser,
optoelectronics, solar cells, nano sensors, nano phosphors, biological markers and so on. In the present
work, ZnS and ZnS:Mn2+ nanoparticles have been synthesized employing a very simple eco-friendly
chemical precipitation technique. For this synthesis, zinc acetate and sodium sulphide were used as the
precursor and manganese acetate as the source of impurity with varying concentration in the presence of
N-N dimethyl Formamide as the reaction catalyst. Deionised water was used as the solvent throughout the
experiment. The structure and optical properties of synthesized nanoparticles were characterized by means
of XRD, FTIR and diffused reflectance spectra. X-ray diffraction analysis confirms cubic zinc blend phase
with no any secondary phase for pure and incorporated with Mn2+ZnS nanocrystals. The average crystallite
size as computed to be around 2.7-4.7 nm range. The crystallite size show decrement with the addition of
Mn2+ impurity. The chemical species of the synthesized crystals are identified by FTIR spectra. Diffused
reflectance spectra show increment in the optical band gap from 3.83- 4.03 eV with the increase in doping
concentration of Mn2+.

Keywords: ZnS:Mn2+, chemical precipitation, XRD, FTIR, DRS, Optical band gap

I. INTRODUCTION
Over the past two decades, a great deal of attention has been devoted into the preparation and characterization of high-
quality nanosized semiconductor nanocrystals as a class of condensed matter with reduced dimension in the nanometre
range, owing to their remarkable physical, chemical, optical, electrical, electronic and catalytic properties which might
have promising potentials in many applications, such as light emitting diodes, lasers, luminescent nanocomposites,
diagnostic agents in medicine, solar cell, phosphors in flat panel displays, cathode ray tube (CRT) and so on [1-3]. ZnS
is an interesting host material of II-VI group semiconductor, which has a wide band gap 3.7 eV at room temperature. It
is one of the versatile and talented phosphor materials which show a variety of luminescence properties, suitable for
applications in the flat panel displays, solar cell, cathode ray tube (CRT), infrared windows, sensors, lasers and so on
[4-6]. Doping on ZnS with transition metal ions like Mn2+and Cu2+ is an important aspect to yield different
nanostructures. Nobel luminescence characteristics such as stable light emission with different colours have been
observed from doped ZnS nanocrystals at room temperature. The impurity ions act as the recombination centres for the
excited electron-hole pairs and results in strong and characteristics luminescence [7-8]. In doped compound
semiconductor, the impurity state plays a very crucial part to affect the electronic energy structures and the transition
probabilities. The quantum confinement impact in the energy states also generates unbelievable physical and optical
features [9]. For the effective preparation of undoped and doped ZnS with transition metals as a representative of a wide
band gap semiconductor nanocrystals, various synthetic techniques have recently been reported by many researchers,
such as sol-gel, chemical precipitation, microwave irradiation, chemical vapour deposition, hydrothermal synthesis and
so on [10-13]. Investigation of ZnS doping with transition metals Mn, Cu, Fe and Ni has been in full swing, as the
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solubility limit for the transition metals is high in II-VI host lattice. Nevertheless, the theoretical and experimental
research on Mn doped ZnS are still limited.
In view of the above discussion, we tried to focus on the synthesis, structural and optical behaviour of Mn2+ doped ZnS
nanoparticles by changing doping concentration. Our main purpose is to investigate the influence of Mn2+ incorporation
on the structural and optical performance of ZnS nanoparticles synthesized by a simple and low cost chemical
precipitation route. The prepared samples have been characterized by XRD, FTIR and UV-Visible DRS Spectrometer.

II. MATERIALS AND METHODS

2.1 Experimental
Pure ZnS and ZnS:Mn2+nanoparticles have been prepared by a chemical precipitation route, using zinc acetate
[(CH3COO)2 Zn, 2H2O] (extra pure Merck), manganese (II) acetate [(CH3COO)2 Mn, H2O](Merck) and sodium
sulphide [Na2S, H2O] (extra pure Loba Chemie) as the starting materials. DMF(CH3)2NC(O)H (Merck) is used as a
stabilizing agent and also the reaction catalyst. All the chemicals used in this investigation were of analytical reagent
(AR) grade and used as received without further refinement. The double distilled water as the solvent for all the
solutions was used in this investigation throughout the experiment.

Figure 1: Flowchart of the synthesis of ZnS:Mn2+ Nanoparticles

2+
ZnS:Mn powder samples were prepared by the chemical route using their acetate salts as follows. First, 0.1 M zinc
acetate [Zn2+] solution was made by dissolving zinc acetate in 100 ml double distilled water and 0.1 M sodium sulphide
[S2-] was also made in 100 ml double distilled water separately. Then 2, 5, 10 and 15 at % manganese (II) acetate
[(CH3COO)2 Mn, H2O] is simply added to zinc acetate solution and stir continuously to mix the solution. Then
appropriate amount of DMF is added in the mixture and stir for 20 minutes. After wards, 100 ml sodium sulphide
solution was added in the mixture drop by drop with constant stirring for 3H. The resulting solution was settled down to
form the precipitate overnight. Later on, it was centrifuged and washed several times with double distilled water and
acetone to get rid of the un-reacted molecules. The obtained precipitate was filtered, dried in vacuum oven at 600C for 8
H. The samples then crushed into a fine powder and then collected in a sample bottle for the characterizations. Pure
ZnS sample also have been prepared in the same manner without impurity material.

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2.2 Characterization of ZnS:Mn2+ Nanoparticles
The structural investigation of ZnS and ZnS:Mn2+ nanoparticles were carried out using X-ray powder diffractometer
(Model: D-8 Advance) with CuKα radiation (λ = 0.15406 nm) scanning 2θ in the range 100- 800. The X-rays were
produced using a sealed tube and the wavelength of X-ray was 0.1541 nm. The X-rays were identified using a fast
counting detector based on Silicon strip technology (Bruker Lynx Eye detector). FTIR spectra were recorded using
Bruker, Germany. Model: Vertex 70 with resolution 0.5 cm-1. UV-Vis diffused reflectance spectra were recorded using
double beam UV-Vis-NIR spectrometer, Make: Perkin Elmer, USA; Model: Lambda 950.

III. RESULTS AND DISCUSSION

3.1 X-ray Diffraction:
XRD is a non-destructive method exploited to characterize the phase and the structure of the nanoparticles. The X-ray
diffraction pattern for pure ZnS and Mn2+ incorporated ZnS nanocrystals with varying Mn2+ (2, 5, 10 & 15%)
concentration at room temperature are depicted in Figure 2.

Figure 2: XRD pattern of ZnS and ZnS:Mn2+ nanoparticles

Analysis of the XRD pattern for pure and doped with Mn2+ ions shows three major peaks in diffractrogram at 2θ values
around 2θ = 28.87°, 48.03°, & 56.81°. It could be easily assigned to reflections from (111), (220) and (311) crystal
planes which reveals that the synthesized products exhibited cubic (zinc blend) lattice structure for all the samples
which matches with the standard JCPDS database (80-0020). The most intense peak of the synthesized products at 2θ =
28.87° is the characteristics of cubic (111) plane [14].
No other diffraction peaks from Manganese impurity were detected upon incorporation of Mn2+ impurity to ZnS host,
which confirms the highest purity of synthesized product and also, the cubic phase of ZnS host remains unaffected due
to Mn2+ substitution because of Zn2+ (0.74 Ǻ) and Mn2+ (0.67 Ǻ) had approximately similar ionic radii [15]. The
diffraction peaks are broadened with Mn2+ substitution representing decrease of crystallite size with Mn2+ incorporation
and the nanosized formation of ZnS. The peak broadening in the diffraction pattern is a due to the presence of the
nanocrystalline character of the particles. The sharp and the intense peaks suggest that the nanoparticles are well
crystallized. Further, the relative intensities of (111), (220) and (311) diffraction are seen to be varied in Mn2+
incorporated ZnS nanoparticles. This might occur due to replacement of Zn2+ by Mn2+ at different lattice sites of ZnS
[16]. The mean crystallite size for all the samples has been computed using Debye-Scherer formula for (111) reflection
in the X-ray diffraction pattern from Full Width at Half Maximum (FWHM). Debye-Scherer formula for the
computation of crystalline size is given by [15]
.
= (1)
Where λ = 0.1541 nm is the wavelength of X-ray diffraction, β is the FWHM in radian of the highest intensity peaks
and θ is the Bragg’s angle.
The average crystallite size of the as-prepared samples estimated using Debye-Scherer formula decreases with the
addition of Mn2+ impurity and found to be lying in the range of 3 - 5 nm
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The lattice parameter ‘a’ for ZnS and ZnS: Mn2+ nanoparticles has been computed using [17] equation 2
= ×√ + + Å (2)
The d-spacing for cubic system for 2θ(111) has been computed by using [15, 18-19] equation 3
= Å (3)
The microstrain determined using [20] equation 4
= (4)
The dislocation density (δ), defined as the length of dislocaton lines per unit volume has been estimated using [20-21]
equation 5
= (5)
The calculated structural parameters of the prepared products are tabulated in Table 1
Table 1: Structural parameters of ZnS and ZnS:Mn2+ nanoparticles
Samples Peak FWHM Particle Lattice Unit Cell Micro Dislocatio d spacing
position (β) Size D paramete Volume strain n Density A0
2θ(111) (degree) (nm) r a3 (ε) (δ) (10-14 for 2θ(111)
(degree) (a) Å lines/cm2)
ZnS (Pure) 28.80 1.7570 4.7 5.3659 154.5 0.4255 0.0453 3.0981
ZnS:Mn(2% ) 28.89 2.5519 3.2 5.3508 153.2 0.6178 0.0977 3.0891
ZnS:Mn (5%) 28. 48 2.6899 3.04 5.4270 159.8 0.6518 0.1082 3.1332
ZnS:Mn 28.89 2.9036 2.8 5.3508 153.2 0.7030 0.1276 3.0891
(10%)
ZnS:Mn 28.74 2.9942 2.7 5.3767 155.4 0.7251 0.1372 3.1042
(15%)

3.2 FTIR Analysis

Fourier Transform Infrared (FTIR) analysis was performed to identify the characteristic functional groups of prepared
samples of the undoped and Mn2+ doped ZnS nanoparticles at room temperature in the wave number range 400-4000
cm-1 and is represented by Figure 3. The FTIR spectra of prepared ZnS and ZnS:Mn2+ samples were carried out by
mixing the samples with KBr in the pellets form.

Figure 3: FTIR spectrum of ZnS and ZnS:Mn2+ nanoparticles

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Analysing the FTIR spectra of ZnS incorporated with different Mn2+ dopant content shows almost similar peaks. It can
be seen that the broad absorption band appeared in the higher energy region of the spectra around 3406 cm-1
corresponds to characteristics vibration band due to adsorbed atmospheric moisture and is ascribed to the stretching
mode frequency of O-H group [22-23]. The peak centred at 1560 cm-1 is attributed to C-O stretching mode vibration
arising from the adsorption of atmospheric CO2 on the surface of the sample [24]. Thepeak appeared at 1404 cm-1 may
be formed by the microstructure of the sample [25]. The peaks occur at 1021 cm-1 and 1099 cm-1 are attributed to
symmetric and asymmetric stretching [26]. The strong peak centred at 481 cm-1 and 666 cm-1 which have been assigned
to vibrations of Zn-S bond [22, 27-28] (i.e. corresponding to sulphides).

3.3 Optical analysis of ZnS and ZnS:Mn2+ Nanoparticles

UV-Visible spectroscopy is a versatile technique to examine the optical performance of the semiconducting
nanomaterials. Measurement of diffused reflectance by employing UV-visible spectrophotometer is a benchmark
method for the investigation of the absorption behaviour of materials. In the case of semiconductor nanocrystals the
most dramatic property that can potentially be estimated from the diffused reflectance are the optical band gap energy,
the energy separation between the field valence band and the empty conduction band. The optical excitation of
electrons across the band gap is firmly endorsed giving rise an unexpected enhances in absorption at the wavelength
analogous to the band gap energy. This aspect of the optical spectrum is known as the optical absorption edge [29].
Estimation of the energy band gap from the measurement of the diffused reflectance of a powder sample is a standard
technique [30]. Hence, UV-Visible diffused reflectance spectroscopy (DRS) has been employed to study the influence
of Mn2+ substitution on the optical performance of nanosized ZnS particles. It allows us to estimate the optical band gap
of the synthesized samples. All the DRS spectra of as synthesized pure and Mn2+ incorporated ZnS samples measured
over the spectral region 200-850 nm with respect to BaSO4 as the reference sample is demonstrate in Figure 4.
From the DRS spectra, as the concentration of dopant material increased the reflectance has been observed to be
reduces slightly in comparison with the undoped sample. The DRS spectra are slightly moved to the lower wavelength
region. Pure ZnS shows band edge absorption at 324 nm. Due to the incorporation of Mn2+ impurity concentration (2, 5,
10 & 15%) undoubtedly show that the band edge absorption move to lower wavelength region with respect to undoped
ZnS sample from 324 nm to 322 nm, 319 nm, 315 nm and 308 nm respectively. The absorption edge of all the
synthesized products shows blue shift with respect bulk ZnS (334 nm) [30] as a result of quantum confinement cause in
the prepared samples. Furthermore, quantum confinement effect takes place owing to the reduction in particle size with
respect to the bulk materials which modify the band gap values.
The computation of the optical band gap values for all the fabricated products has been done employing diffused
reflectance spectra (DRS) according to the Einstein’s well known energy wavelength equation [28, 31]
= (6)
For undoped ZnS, the value of optical band gap has been computed to be 3.83 eV. The estimated values of the optical
band gap show increment in its values due to the addition of Mn2+ dopant content. The optical band gap values for Mn2+
(2, 5, 10 & 15%) inserted ZnS products were computed from DRS spectra to be 3.85 eV, 3.89 eV, 3.94 eV and 4.03 eV
respectively and are listed in Table 2. The results show increment in the optical band gap values of the synthesized
product due to the insertion of the Mn2+ doping concentration resulting in to the reduction in particle size due to the
quantum confinement impact.
The particle radius of all the synthesized products is computed according to the mathematical model of effective mass
approximation by means of [32-33] equation 7.
. . √ .
( )= (7)
( . )
Where, r is the particle radius (2r is the diameter and hence the particle size) and E is the optical band gap energy. The
optical band gap and the average particle size of undoped and Mn2+ doped ZnS nanoparticles have been estimated using
equation (6) and (7) and are summarized in Table 2.

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Figure 4: Diffused Reflectance spectra of ZnS and ZnS:Mn2+ Nanoparticles

Table 2: Optical parameters of ZnS and ZnS: Mn2+ samples.
Samples Absorption Band gap Crystalline
edge λ (nm) Eg (eV) size (nm)
ZnS 324 3.83 4.12
ZnS:Mn(2%) 322 3.85 4.04
ZnS:Mn(5%) 319 3.89 3.88
ZnS:Mn(10%) 315 3.94 3.68
ZnS:Mn(15%) 308 4.03 3.4
The values of the band gap summarized in the above Table 2 are larger than the bulk band gap of ZnS (3.7 eV) on
account of quantum confinement impact.

IV. CONCLUSIONS
2+
In summary, ZnS and ZnS:Mn nanoparticles, sizes in the range of 3 – 5 nm were successfully synthesized by
chemical precipitation method. The structural characterization done through XRD exhibits cubic phase crystal structure
for all the prepared samples and no any characteristic peaks of manganese impurity were detected, at least within the
resolution limit of the diffractometer. The particle sizes of the prepared samples are found to be decreasing with the
addition of Mn2+ doping content. The UV-Visible DR Sspectrum shows that the optical band gap of the prepared
samples increases with Mn2+impurity concentration due to quantum confinement effect. The functional groups of ZnS
and ZnS:Mn2+ nanoparticles are determined by FTIR study. FTIR analysis reveals the Zn – S stretching at 481 and 666
cm-1. Thus the prepared material has a good potential to be used in solar cells and optoelectronic devices applications.

ACKNOWLEDGEMENT
The authors are grateful to the centre director, UGC-DAE Consortium for Scientific Research Centre, Indore for
providing the facilities. The authors are thankful to Dr. Mukul Gupta for XRD, Dr. U. P. Deshpande for FTIR and DRS
measurements.

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