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Article history: This work reports the structural, morphological and optical properties of zinc sulphide (ZnS) thin lms
Received 28 March 2015 obtained by chemical spray pyrolysis (CSP) technique using zinc chloride as cationic and thiourea as
Received in revised form anionic source with ethylene-diamine tetra acetate (EDTA) complex. The ZnS thin lms were deposited
4 July 2015
on glass substrate at 300 C, 400 C and 450 C. The inuence of the substrate temperatures on the
Accepted 19 July 2015
Available online 21 July 2015
structural, morphological and optical properties was studied. The XRD spectra show that the lm is
nanocrystalline with peak intensity increasing with temperature. The morphology of the lms was seen
by scanning electron microscopy (SEM). The lms dislocation density and micro strain increased with
Keywords:
Spray pyrolysis method
temperature. Optical properties show a high transmittance which increased with temperature.
Zinc sulphide 2015 Elsevier B.V. All rights reserved.
Optical properties
Structural properties
http://dx.doi.org/10.1016/j.jallcom.2015.07.169
0925-8388/ 2015 Elsevier B.V. All rights reserved.
382 P.O. Offor et al. / Journal of Alloys and Compounds 650 (2015) 381e385
lms on glass substrates were prepared by spray pyrolysis tech- complex at substrate temperatures of 300 C, 350 C, 400 C and
nique at 220, 250 and 280 C. Aqueous solution of 50 ml containing 450 C.
zinc acetate dehydrates and thiourea salts of 1:1 M were used [16].
Also Zns thin lms were deposited by chemical spray pyrolysis 2. Experimental details
(CSP) using mixed aqueous solutions of zinc sulphate and thiourea
at substrate temperature of 500 C [17]. Zns thin lms were also Thin lms of zinc sulphide were deposited on glass substrates
prepared using zinc chloride and thiourea by spray pyrolysis at (7.5 2.5) cm2 by chemical spray pyrolysis (CSP) equipment
substrate temperature of 400 C [18]. Zns thin lms were suc- developed in the Department of Metallurgical and Materials Engi-
cessfully deposited on glass substrates by CSP method using zinc neering, University of Nigeria, Nsukka. The glass substrates were
acetate and thiourea at substrate temperature range of 300e400 C washed with detergent, rinsed in water, rinsed in distilled water,
[7]. In the same vein Zns thin lms were prepared by CSP using two soaked in acetone for 20 min to remove contaminants and rinsed
mixed aqueous solutions: (a) dehydrated zinc acetate (102M) and again in distilled water. After the cleaning process, the substrates
thiourea (4 102 M) in bidistilled water; (b) Zinc chloride were placed on a tray and dried in a sterilizer (oven). The deposition
(102 M) and thiourea (4 102M) in bidistilled water. The solu- process involved the thermal decomposition of an aqueous solution
tions were sprayed on silica gel substrates heated to 500 C for rst of zinc salt, thiourea and ethylen-diamine tetra acetate (EDTA. Zinc
solution and 450 C for the second [1]. Zns thin lms were prepared chloride (ZnCl2) was used as the of Zn2 ion, thiourea (SC(NH2)2) as
by CSP using zinc chloride, thiourea and drops of hydrochloric acid the source of S2 ion and EDTA (C10H16N2O) was added as a com-
on glass substrates heated to a temperature of 350 C [19]. Boron plexing agent. Solution containing zinc chloride (ZnCl2), and thio-
doped Zns thin lms were deposited on highly clean glass sub- urea (SC(NH2)2) of molar concentration 0.1 M and EDTA of molar
strates at different temperatures within the substrate temperature concentration 0.01 M were used to prepare zinc sulphide (ZnS) thin
rage (450e550 C) by CSP. The starting materials used were zinc ims. The equation of reaction is as follows:
chloride, thiourea and boric acid [3]. Nanoparticle Zns lms were
deposited on glass substrates by CPS at temperature of (400 5 C). ZnCl2aq SCNH2 2aq 2H2 O/ZnSs 2NH3aq CO2g
The lms were annealed at 450, 500, 550 and 600 C. The spraying
2HClg
solution was prepared by mixing zinc chloride and thiourea as
starting materials [20,21]. Zns thin lms were deposited on the (1)
glass substrates at 350 C by CSP and annealed at 450 C and 550 C.
The time interval between two sprays was kept constant at 10 s.
An aqueous solution of zinc acetate and thiourea were used to
The spray pressure and the spray nozzle to substrate distance were
deposit the Zns thin lms [12]. The present study reports the
kept constant at 4 bars and 20 cm respectively. The ZnS thin lms
preparation of zinc sulphide thin lms on glass substrates by a
were deposited on the glass substrates at 300 C, 350 C, 400 C and
chemical spray pyrolysis equipment using 0.1 M zinc chloride, 0.1 M
450 C respectively.
thiourea and 0.01 M ethylene-diamine tetra acetate (EDTA)
Structural study was done using EMPYREAN X-ray
Table 1
Variation of interplanar distance, FWHM, hkl, dislocation density and micro strain values with substrate temperature for the ZnS thin lms.
Temperature ( C) 2q d spacing () D ASTM () FWHM (b) (hkl) Standard Lattice Crystalline size(G) Dislocation density (d) Micro strain ()
constant (a) () (nm) (Lines/m2) 1015 102
300 27.04 3.3 3.32 0.055 002 3.8 25.96 1.4839 1.3369
43.86 2.1 1.904 0.058 110 3.8 25.96 1.4839 1.3451
56.26 1.6 3.12 0.060 118 3.8 25.96 1.4839 1.3228
350 28.52 3.1 3.32 0.057 002 3.8 25.12 1.5847 1.3811
61.00 1.5 3.12 0.064 118 3.8 25.12 1.5847 1.3786
400 26.49 3.3 3.16 0.057 008 3.8 23.03 1.8854 1.3871
41.73 2.2 3.20 0.066 102 3.8 23.03 1.8854 1.5418
53.22 1.7 2.93 0.069 104 3.8 23.03 1.8854 1.5423
71.86 1.3 1.904 0.076 110 3.8 23.03 1.8854 1.5385
450 25.64 3.5 3.32 0.077 002 3.8 18.47 2.9313 1.8770
diffractometer system. X-ray diffraction spectra were obtained us- electronic and optoelectronic devices [25]. The existence of multi-
ing CuKa (l 1.5406 ) radiation. Surface morphology was studied ple diffraction peaks in the diffraction patterns indicated poly-
using JOEL JSM 5900LV scanning electron microscope (SEM, and the crystalline nature with hexagonal structure for the ZnS lms. The
optical properties were measured by Avantes UVeVISeNIR (002) peak has pronounced intensity with temperature. It is highest
spectrophotometer. at 450 C. The d-values were calculated from the peaks of the X-ray
spectrum using Bragg's relation [18]:
the substrate with very at surface. The lms contain cracks and
voids which grow with increase in temperature.
4. Conclusions