Phase-dependent thermoluminescence properties of zinc sulphide

doi:10.21203/rs.3.rs-5180178/v1

In the current study, the effects of heat treatment on the thermoluminescence (TL) and structural properties of zinc blend samples were studied. The samples were annealed after being heated for different time periods from 2 up to 10 hours. The wurtzite hexagonal phase was observed upon heat treatment; however, its percentage decreased with the treatment period. The morphology of ZnS particles was studied by the HR-TEM analysis and it displayed an aggregated ZnS nanoparticles with almost uniform shape and size. The TL-glow curves for each sample were analysed using the CGCD method. Six trapping peaks exist between 0.98 and 1.45 eV through the deconvolution of the glow curves. The number of peaks were increased to 8 peaks for the fourth treatment, located between 0.95 and 1.56 eV. The activation energies and the frequency factors for getting traps were evaluated.

Zinc sulphide

Thermoluminescence

XRD

Thermal treatment

Activation energies

Recent years have seen a significant amount of interest in semiconductor nanomaterials having luminous properties due to their potential use in optoelectronic devices, light emitters, and solar cells. Among these materials, zinc sulphide is considered a promising material that can be utilized for various applications in optical devices such as light-emitting diodes, lasers, flat-panel displays, infrared windows, sensors, and photocatalysts [1, 2]. Zinc sulphide has two stable phases: a cubic zinc blend (ZB) phase and a hexagonal wurtzite (WZ) phase. Both phases are of industrial importance; however, the more stable polymorph is the cubic phase under ambient conditions because of its free energy difference of ∼10 kJ mol^− 1. The ZB structure's bandgap is 3.68–3.72 eV, whereas the WZ phase's is 3.77 eV [1]. The hexagonal polymorph of the ZnS possesses much attention since its luminescent properties are considerably superior to the cubic phase. Therefore, the hexagonal wurtzite structure is preferable in optoelectronics applications [3].

Under the exposure of ionizing radiation, free electrons or holes were created and may be trapped by some defects or centres inside the material. If these traps are energetically deep enough, the trapped carriers may remain stable for a period, unless they are freed by external stimulation. The thermally stimulated light emission is commonly referred to as the thermoluminescence (TL) property of this material. One of the most widely used techniques for studying optical properties is thermo-stimulated luminescence (TL); it is based on creating traps to catch the charge carriers moving to/from the conduction band. As electrons gain energy from radiation and are excited by the conduction band, charge carriers will get caught by the defect traps in the crystalline structure. TL phenomena are present in several naturally occurring minerals, such as muscovite [4], quartz [5–7], feldspar [8], fluorapatite [9], and calcite [10, 11]. This property can be induced synthetically by adding rare elements and few metals to the host material [12–15]. There are various reports of nano-zinc sulphide phase transformation from its cubic to wurtzite phase by annealing [16, 17]. Any change in the crystal structure is of great importance and would influence the TL glow curves [18, 19].

The current work was going to study the heat treatment effect on the zinc sulphide phase transformation and crystal structure and its influence on luminescence properties and optical sensitivity.

The zinc sulphide phase was prepared by using the simple chemical co-precipitation method at room temperature, both zinc sulphate [ZnSO₄.xH₂O] and sodium sulphide [Na₂S.xH₂O] were used as starting materials to get raw zinc and sulphur. To achieve complete dissolution, 71.9 gm and 19.5 gm of zinc sulphate, and sodium sulphide, respectively, were dissolved in 250 ml of distilled water at room temperature and stirred for 15 minutes. The mixture of the homogeneous solutions of zinc sulphate and sodium sulphide was placed on a magnetic stirrer for 3 hours with continuous stirring at room temperature. The mixture of solutions was kept at room temperature for 24 hours before being filtered. The precipitated material was filtered and washed by distilled water several times and then allowed to dry in an oven (120°C) for 6 hours.

The prepared samples were exposed to beta particles at doses ranging from 0.11 Gy to 330 Gy. The irradiation process was carried out using an automated Lexsyg Smart TL/OSL luminescent reader with a built-in source of the ⁹⁰Sr/⁹⁰Y at a dose rate of 0.11 Gy/s and a maximum energy of 2.2 MeV. The glow curves of the prepared samples were deconvoluted using new TL software [20] developed in the Lab of Nuclear Radiation Measurements at the Department of Physics, Faculty of Science, Ain Shams University, Cairo, Egypt.

The texture and morphological properties of the samples were studied using high-resolution transmission electron microscopy (HR-TEM) Talos F200i (FEI, USA) microscope operating at 200 kV. The crystal structure of the samples was studied by x-ray diffraction method (XRD) using an X-ray diffractometer by PANalytical (Model-X'Pert Pro) with CuK_α irradiation of wavelength 1.54060 Å with operation voltage of 40 kV and current of 40 mA in a scanning range (2θ) of 20^ο − 70^ο. All the data as well as the blank sample were studied and fitted using Rietveld refinement using the FULLPROF suite [21, 22].

3.1. Morphological and structural analysis

The morphology and structure of ZnS particles were studied by the HR-TEM analysis and XRD. The TEM images of the heat-treated samples in Fig. 2 (b-e) displayed an aggregated ZnS nanoparticles with almost uniform shape and size. It can be observed that the particles are close to the spherical shape, which in turn confirms the new hexagonal phase formation as determined from x-ray diffraction data. At a higher magnification, the lattice spacing of the hexagonal ZnS can be observed for the heat-treated samples, whereas the unannealed sample image (Fig. 2a) shows an aggregated plate-like morphology [23].

There are two widely accessible phases of zinc sulphide (ZnS): a zinc blend (ZB) phase and a wurtzite (WZ) phase. In both structures, Zn and S atoms have 4:4 arrangements and are tetrahedrally bonded, but they differ only in the stacking sequence [24]. In zinc blende, the S forms cubic close packing with Zn in the ABCABCA… arrangement, while in the wurtzite phase, the sulphide ions have a hexagonal close packing of ABABAB…... [22]. The cubic phase is the stable one at low temperatures and crystallizes in the face-centered cubic space group F-4 3 m. The Rietveld refinement of the XRD data for the pure phase confirms this cubic structure for the unannealed zinc sulphide, as shown in Fig. 4 (a, b).

The results of the X-ray diffraction data show that the unannealed ZnS sample (blank) crystallized in a cubic phase structure with a lattice parameter of 5.3486 (13) (Å). The XRD peaks of the cubic phase are broadened due to the nanocrystalline nature of the synthesized sample. The unannealed sample average grain size was calculated using Scherrer Eq. (1), taking into consideration the instrumental contribution [25], and was found to be 187.2 (7) nm.

$$\:L=\:\frac{k\:\lambda\:}{\beta\:\:\text{cos}\left(\theta\:\right)}$$

1

Where L is the crystallite size, λ is the wavelength used, β is the integral breadth after correcting the instrument peak broadening (β expressed in radians), and the constant k is a function of the crystallite shape.

It can be observed from the x-ray diffraction data that there are observable additional peaks as well as a change in those peaks’ intensities upon heat treatment. There is an observed peak found at 26.9^ο that corresponds to the (100) peak of the hexagonal phase (Fig. 3). The XRD data shows that the hexagonal phase percentage tends to decrease as the heat treatment period increases from two to eight hours, as seen in Fig. 3 inset. The area percentage for the hexagonal peaks decreases from 12.6% for the 2 hrs annealed sample to 8.2% for the 8 hrs annealed samples. However, the hexagonal phase shows no significant decrease for samples treated for four and six hours, and the hexagonal peak area percentages were 11.6% and 11%, respectively.

3.2. Thermal treatment effect

Zinc sulphide (ZnS) powder samples were synthesized and subjected to thermal treatments to increase their TL sensitivity. The powder samples had four different thermal treatments for two, four, six, and eight hours at 500^oC. Zinc sulphide powder TL glow curves for all four thermal treatments and for the powder without any heat treatment (blank sample) are shown in Fig. 4 (a). Regarding the four different heat treatments, it was noticed that the low TL intensity of the light curve was untreated, and up until the fifth one, TL behaved like it was growing up, then decreased again in the fifth treatment. This indicates that the mixture of both phases increased the luminescence properties, and the best TL intensity was for the 8.2% hexagonal and 91.8% cubic phase, as presented in Fig. 4(b). For every thermal treatment, the total area beneath the produced glow curves is shown in Fig. 5(b). Samples of zinc sulphide (ZnS) powder without heat treatment had the lowest behaviour progressively improving towards the third treatment. According to the figure, the fourth thermal treatment had the highest intensity. For in-depth examinations of the TL characteristics and evaluations of the kinetic parameters, samples of powder zinc sulphide that underwent all thermal treatments will be chosen.

3.3. Glow curve analysis and kinetic parameters

The activation energies of each of the distinct peaks and their supplemental frequency factors were derived from the deconvolution analysis executed on the TL-glow curves using the newly TL software given by El-Kinawy et al. [20]. The CGCD method is based on the general-order kinetics model, The following is the glow curve deconvolution equation:

$$\:I\left(T\right)={I}_{M}\text{exp}\left(\frac{E}{k\:T}\left(\frac{T-{T}_{M}}{{T}_{M}}\right)\right)\times\:{\left[1+\frac{E\left(b-1\right)\left(F\left(T,E\right)-F\left({T}_{M},E\right)\right)}{k\:{T}_{M}^{2}\:b\text{exp}\left(\frac{-E}{k\:{T}_{M}}\right)}\right]}^{\frac{-b}{b-1}}$$

2

Here, the parameters I_M and T_M refer to the maximum intensity of the glow peak and the corresponding temperature, respectively. The optimization parameter E (eV) represents the thermal activation energy of the corresponding carrier trap, b is the order of kinetics, T (K) is the absolute temperature, and k (J/K) is the Boltzmann constant (8.617E-5 eV/K).

The two functions $\:\text{F}\left(\text{T},\text{E}\right)$ and $\:\text{F}\left({\text{T}}_{\text{M}},\text{E}\right)$ are given by,

$$\:F\left(T,E\right)=T\text{exp}\left(\frac{-E}{k\:T}\right)+\:\frac{E}{k}\left(Ei\left(\frac{-E}{k\:T}\right)\right)$$

3

$$\:F\left({T}_{M},E\right)=T\text{exp}\left(\frac{-E}{k\:{T}_{M}}\right)+\:\frac{E}{k}\left(Ei\left(\frac{-E}{k\:{T}_{M}}\right)\right)$$

4

Such that, Ei(-x), with x > 0, is the exponential integral function [26]

The frequency factor (s) be computed after that using the equation below:

$$\:s=\:\left(\frac{E\:\beta\:}{{k\:T}_{M}^{2}}\right)\frac{1}{1+(b-1)\left(\frac{2\:k\:{T}_{M}}{E}\right)}\text{exp}\left(\frac{E}{k\:{T}_{M}}\right)$$

5

The figure of merit (FOM) that Eddy and Balian created [27]:

	$\:FOM=\sum\:_{{j}_{i}}^{{j}_{f}}\frac{100\:({y}_{j}-y({k}_{f}\left)\right)}{A}$	(6)

The following channels represent the region of interest: j_i for the first channel, j_f for the final, y_j for the information for the content of channel j, y(k_f) for the fitting function in channel j, and A for the integral in the interest region of the fitted glow curve.

The zinc sulphide sample produced without thermal treatment (blank) and the sample that received a fourth thermal treatment after being subjected to 1.0 KGy had their TL glow curves deconvoluted using the CGCD method. The sample that was not heat-treated showed six overlapping peaks, as shown in Fig. 5(a). After undergoing the first and second thermal treatments, the resulting zinc sulphide sample was exhibited in Fig. 5(b, c) with seven overlapping peaks. For the third and fourth treatments, the number of peaks climbed to eight overlapping peaks, as seen in Fig. 5(d, e). Table 1 provided the average values of the kinetic parameters, E (eV), T_M (K), s (s^− 1), and b for the sample without the thermal treatment and for all the fourth thermal treatments. A radiative transition occurs when a trapped charge carrier is liberated from the matching trap, and we refer to this energy as the activation energy (E). The frequency factor called the attempt-to-escape factor (s) is linked to the possibility of the trapped charge carriers being thermally freed. The first, second, or general-order behaviour of the trapping center is indicated by the order of kinetics (b).

As a result, it was established that only six locations of the produced zinc sulphide sample without thermal treatment for TL components were 358.5, 376.2, 405.3, 431.7, 513.3, and 547.8 K. After undergoing the first thermal treatment, the peak position from one to six exhibits a shift toward the low temperature and appears to peak at 529.9 K. The second treatment's impact was a change in the peak position to the side with lower temperatures and still seven positions. In addition to creating eight peak locations in the third thermal treatment, additional thermal treatment resulted in the peak site migrating to a lower temperature, with peak eight emerging at 545.7 K. The fourth thermal treatment results in the eight peak positions appearing as well, with significant effort shifting in the peak locations to be 356.1, 364.4, 389.4, 420.7, 448.6, 478.7, 508. 5, and 528.9 K.

Table 1

Kinetic parameters of the prepared zinc sulphide samples from the CGCD method before thermal treatment and for all the fourth thermal treatment.
		P1	P2	P3	P4	P5	P6	P7	P8
before thermal treatment	Tm (K)	358.5	376.2	405.3	431.7	513.3	547.8
	E (eV)	0.98	1.04	1.17	1.31	1.34	1.46
	s (s^− 1) * 10¹⁴	0.283	0.312	0.0792	8.3	4.2	1.23
	b	1.53	1.69	1.72	1.71	1.55	1.44
1st thermal treatment	Tm (K)	358.2	375.3	403.3	430.9	460.1	502.9	529.9
	E (eV)	1.00	1.05	1.19	1.30	1.36	1.44	1.55
	s (s^− 1) * 10¹⁴	2.6	0.559	2.29	2.25	0.465	10.01	1.87
	b	1.42	1.62	1.82	1.59	1.36	1.51	1.40
2nd thermal treatment	Tm (K)	357.5	373.7	402.4	424.7	455.6	489.8	516.2
	E (eV)	1.02	1.04	1.17	1.29	1.31	1.47	1.54
	s (s^− 1) * 10¹⁴	0.855	0.683	1.67	2.59	2.42	20.42	3.19
	b	1.51	1.63	1.84	1.57	1.37	1.52	1.42
3rd thermal treatment	Tm (K)	357.2	370.94	390.1	422.7	451.0	480.5	489.7	545.7
	E (eV)	0.99	1.01	1.16	1.29	1.31	1.41	1.49	1.57
	s (s^− 1) * 10¹⁴	0.446	3.28	4.04	4.07	5.94	10.03	7.82	0.237
	b	1.52	1.59	1.84	1.59	1.31	1.51	1.40	1.41
4th thermal treatment	Tm (K)	356.1	364.4	389.4	420.7	448.6	478.7	508.5	528.9
	E (eV)	0.95	1.01	1.14	1.31	1.36	1.42	1.51	1.56
	s (s^− 1) * 10¹⁴	0.0534	0.191	2.11	20.28	7.41	2.90	3.11	6.37
	b	1.55	1.70	1.79	1.00	1.38	1.65	1.37	1.46

Using thermally treated zinc sulphide samples, it was observed that there was a slight shift in locations from peak one to peak three and a significant shift in positions from peak four to peak eight. Finally, heat treatment produced a trap by shifting the trap position to the side with a lower temperature.

The present experiment aims to explore the influence of heat treatment on the luminescent properties and phase transformation of zinc sulphide. The microscopy and x-ray diffraction analysis confirmed the presence of hexagonal structure in the annealed samples in addition to the cubic zinc blend phase. The hexagonal phase was found to decrease from 12.6–8.2% with the increase in heat exposure time. The presence of both phases enhanced the luminescence of the material; however, the best composition for luminescence among the prepared samples was the 8.2% hexagonal phase and 91.8% cubic phase. The TEM images of the heat-treated samples displayed an aggregated ZnS nanoparticles with almost uniform shape and size. It can be observed that the particles are close to the spherical shape, which in turn confirms the new hexagonal phase formation as determined from x ray diffraction data. The TL-intensities indicated extremely higher thermoluminescence properties of thermally treated ZnS than that of the untreated ones. The analysis of the TL signals revealed the composition of the glow curves of the treated for 8 hours at 500^oC of eight TL components revealed higher TL sensitivity than other treatments. So, ZnS samples that treated thermally for 8 hours at 500 ^oC recommended for studying the TL dosimetric properties. In the future, distortion of the hexagonal additional phase could be studied, which in turn will affect the trap concentration found in the band gap and hence study their influence on the structural and spectroscopic properties.

Author Contribution

All authors have seen and approved the final version of the manuscript being submitted. They warrant that the article is the authors' original work, hasn't received prior publication and isn't under consideration for publication elsewhere.

Conflict of Interest

No conflict of interest

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No competing interests reported.

Phase-dependent thermoluminescence properties of zinc sulphide

Status:

Version 1

Abstract

Figures

1. Introduction

2. Material and methods

3. Results and Discussion:

3.1. Morphological and structural analysis

3.2. Thermal treatment effect

3.3. Glow curve analysis and kinetic parameters

4. Conclusions

Declarations

Author Contribution

References

Additional Declarations

Status:

Version 1