Structural and optical properties of nanocrystalline CdS films … · 2017. 10. 16. · CdS films prepared by spray pyrolysis Radhyah M. S. Aljarrah, Adnan H. Aljobory* Department

Available online at www.worldscientificnews.com

WSN 87 (2017) 175-190 EISSN 2392-2192

Structural and optical properties of nanocrystalline CdS films prepared by spray pyrolysis

Radhyah M. S. Aljarrah, Adnan H. Aljobory*

Department of Physics, Faculty of Science, University of Kufa, Box 21 Kufa, Najaf, Iraq

*E-mail address: [email protected]

ABSTRACT

Cadmium Sulphide (CdS) thin films are produced using spray pyrolysis deposition technique.

Films are annealed in air at 400, 500, and 600 K of 1 h. It characterized by X-Ray Diffraction (XRD),

Atomic Force Microscope (AFM) and optical properties of CdS. XRD shows that these films are

polycrystalline in nature with cubic and hexagonal crystalline structure. The crystallite size,

microstrain, and dislocation density were measured. AFM shows that the total substrate surface is

finely covered with uniformly distributed spherical shaped grains. Optical transmittance was shown

that direct transition with band gap energy was decreased between 2.44 to 2.27 eV with annealing.

Keywords: Cadmium Sulphide, CdS films, spray pyrolysis

1. INTRODUCTION

In recent years, semiconductor materials have been growing interest in II-VI for

potential applications in optoelectronic and photovoltaic industries. This compound is a strong

candidate as a window layer in a solar cell because it has a wide direct gap. CdS is a

promising material widely employed in the technology of optoelectronic devices (optical

filters, photodetectors, gas sensors and above all for solar cells) [1-5]

. The basic requirements of

CdS in applications are high optical transparency, wide direct band gap between 2.28 eV and

2.45 eV, high transmittance, stability and low cost, low dark electrical resistivity, high

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photoconductivity and better crystallinity [6-11]

. CdS is a chalcogenide n-type semiconductor.

It is known as CdS thin films may exist in a cubic or in hexagonal phase or as a mixture of

both phases depending on factors including deposition technique [9,12]

. CdS are fabricated

using various techniques (sputtering, chemical vapor deposition, spray pyrolysis, RF

sputtering, pulsed-laser deposition, and chemical bath deposition) [13-17]

. Spray pyrolysis was

suitable for manufacturing CdS is known as the simplest and economical for the large area

productions in obtaining thin films [6-45]

.

2. MATERIALS AND METHODS

Spray pyrolysis method is nanostructured thin-film preparation method with excellent

features such as no need sophisticated equipment and quality targets or substrates. Film

thickness and stoichiometry are easy to control and the resulting films are well compacted.

CdS produced using spraying the aqueous solution of 0.1 M of cadmium acetate (CH3COO)2· Cd·H2O ≡ 266.52 g ml

-1 onto the microscope slide (1×25×25 mm

3) at 350 °C. 50 ml thiourea

was used. Prior to deposition, the substrates were cleaned using cleaner solution, distilled

water, and alcohol using an ultrasonic bath. The spray rate was adjusted to one sprinkling in a

minute, the sprinkling time about of 11 s. The normalized distance between the spray nozzle

and the substrate is 30 cm. The temperature of the substrate was controlled by an Iron-

Constantan thermocouple.

The thickness of the films (t) was determined using weighing-method.

t =

where = Mass difference of slide, A = aria = 2.5×2.5 cm2

and ρ = CdS density = 4.824 g

cm-3

. X-ray with Cu Kα radiation λ = 0.15406 nm was used to investigate the film structure,

the grain size used to CdS was determined by average grain size in the c-axis orientation

estimated using the Debye-Scherrer relation [18]

:

D = 0.9λ / B cos θ

where D = Mean particle size, θ = Bragg diffraction angle and B = Full width at half

maximum (FWHM) of the diffraction peak. The optical absorption test was recorded by using

a Shimadzu UV1650 PC spectrophotometer. The absorbance and the reflectance measured for

the scanning of the electromagnetic spectrum (300-1100 nm). to The energy gap and the

optical constants such as refractive index (n), extinction coefficient (k), real, and imaginary

parts of dielectric constant (ε1and ε2) were measured. The optical energy gap (Eg) was

determined using Tauc Eq: [19,20]

(αhυ) =B (hυ-Eg )r

where B = Tauc constant and hυ = Photon energy, α = Absorption coefficient. R = 1/2,

indicate the direct transition. The optical energy gap of the film obtained by plotting (αhν)2 ~

hν and determination the straight line, and make it extend to meet the energy axis. The optical


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properties of a material are utilized to determine its optical. The extinction coefficient

describes the energy absorption of the electromagnetic wave during the process of

transmission of a wave through a material. The intensity of light (I) after crossing thickness of

material x in an isotropic medium can be estimated by [21,22]

.

I = I0 exp (–αx)

where I0 = Initial intensity. The extinction coefficient k is equal to [21,22]

:

k = αλ/4π

where λ = wavelength. The normal-incidence reflectivity R can also be given by [21,22]

:

Then the refraction index value can be calculated from the formula [21,22]

:

The real and imaginary part of dielectric constant determined:

εr = n2 − k2, εi = 2nk [23]

3. RESULTS AND DISCUSSION

Fig. 1 shows X-ray diffraction patterns of CdS. It was seen that as-deposited CdS has

the mixtures of cubic and hexagonal structures [24]

. It is difficult to distinguish between cubic

(1 1 1) and HCP (0 0 2), cubic (2 2 0) and HCP (1 1 0). After the high-temperature process,

new peaks of hexagonal structure appealed at XRD patterns. This phenomenon was thought to

be the phase change of CdS using heat treatment. It was believed that the mixtures of

hexagonal and cubic phase were changed to hexagonal phase by the heat treatment.

The hexagonal phase of CdS is thermodynamically stable than the cubic phase of CdS [25,26]

. The XRD patterns revealed that highest peaks correspond to the H (0 0 2) C (1 1 1),

(2 2 0), and (3 1 1) phase. It shows a small hexagonal (1 0 0), H (1 1 0), and C (2 2 0) peaks.

The different peaks in the diffractogram were indexed and the corresponding values of

interplanar spacing “d” were calculated and compared with standard values of JCPDS data [27]

.

The annealing resulted in good quality films with improved crystallinity as evidenced by

intense diffraction peaks indicated (Fig. 1). The position of HCP (0 0 2) peak was changed

from 27.21 to 26.81. It may be due to the relaxation of tensile stress. The tensile stress of the

as-deposited CdS developed by lattice mismatch of the hexagonal structure of CdS. Lattice

parameters of hexagonal structure of CdS reported being a = 4.1450 Å and c = 6.721 Å.


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The FWHMs of HCP (2 0 0) peaks and crystalline size (D). It was calculated by

Scherrer’s formula (Table 1). The FWHM and crystalline size (D) of as-deposited CdS are

0.4278 Å and 91.3 nm, respectively. After the high-temperature process, the FWHM and

crystalline size (D) increase, which indicates the grain growth of CdS. These results are

agreement with Mariappan et al, 2012 [28-45]

.

Fig 1. XRD for CdS at different annealing temperature (a-R. T, b-400K, c-500K,

and d-600K).


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Table 1. The peaks observed in all films and the standard peaks from JSPDS [27].

Ta (K) 2θ

(Deg.)

FWHM

(Deg.)

dhkl

Exp.(Å)

D

(nm) Phase hkl

dhkl

Std.(Å) Card No.

R.T

30.6731 0.4278 2.9124 19.3 Cub.

CdS (200) 2.9090

96-900-

8840

43.9820 0.5703 2.0571 15.0

Hex.

CdS (110) 2.0674

96-900-

8863

Cub.

CdS (220) 2.0570

96-900-

8840

400

24.4563 0.5348 3.6368 15.2 Hex.

CdS (100) 3.5808

96-900-

8863

26.7500 0.3922 3.3300 20.8

Hex.

CdS (002) 3.3745

96-900-

8863

Cub.

CdS (111) 3.3590

96-900-

8840

30.5000 0.4520 2.9285 18.2 Cub.

CdS (200) 2.9090

96-900-

8840

44.0420 0.4991 2.0544 17.2

Hex.

CdS (110) 2.0674

96-900-

8863

Cub.

CdS (220) 2.0570

96-900-

8840

48.1000 0.6300 1.8902 13.8 Hex.

CdS (103) 1.9049

96-900-

8863

52.4300 0.4278 1.7438 20.7 Cub.

CdS (311) 1.7542

96-900-

8840

500

24.8841 0.5348 3.5753 15.2 Hex.

CdS (100) 3.5808

96-900-

8863

26.5241 0.5348 3.3578 15.3

Hex.

CdS (002) 3.3745

96-900-

8863

Cub.

CdS (111) 3.3590

96-900-

8840

28.1996 0.5348 3.1620 15.3 Hex.

CdS (101) 3.1632

96-900-

8863


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30.4210 0.3922 2.9360 21.0 Cub.

CdS (200) 2.9090

96-900-

8840

44.0210 0.3921 2.0554 21.9

Hex.

CdS (110) 2.0674

96-900-

8863

Cub.

CdS (220) 2.0570

96-900-

8840

47.8000 0.6540 1.9013 13.3 Hex.

CdS (103) 1.9049

96-900-

8863

52.2100 0.4278 1.7506 20.7 Cub.

CdS (311) 1.7542

96-900-

8840

600

24.6702 0.3921 3.6058 20.7 Hex.

CdS (100) 3.5808

96-900-

8863

26.5600 0.3600 3.3534 22.7

Hex.

CdS (002) 3.3745

96-900-

8863

Cub.

CdS (111) 3.3590

96-900-

8840

28.2709 0.4950 3.1542 16.6 Hex.

CdS (101) 3.1632

96-900-

8863

30.5320 0.4230 2.9256 19.5 Cub.

CdS (200) 2.9090

96-900-

8840

43.9200 0.3460 2.0599 24.8

Hex.

CdS (110) 2.0674

96-900-

8863

Cub.

CdS (220) 2.0570

96-900-

8840

48.0214 0.4500 1.8931 19.3 Hex.

CdS (103) 1.9049

96-900-

8863

52.5300 0.4500 1.7407 19.7 Cub.

CdS (311) 1.7542

96-900-

8840

The Average Surface Roughness (RMS) values and the average surface grain size are

shown in Table 2. These results are agreement with Mazón-Montijo, et al, 2010 [29]

. The grain

size of the film was determined using the AFM, the average grain size increases as increasing

Ta because the increasing Ta can cause recrystallization in grains, leading to a reorientation of

the film and a significant increase in average grain size. Consequently, the surface roughness

increases as increase the grain size.


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Figs. (2a, b, c, and d) shows typical surface using AFM of CdS at 350oC and annealed at

temperatures (400, 500 and 600) K of 1h. All the images show a homogeneous distribution

with columnar structure.

a.. b

c.. d

Fig. 2 AFM images: (a) deposited CdS (b) annealed at 400K, (c) 500 K and (d) 600K.

The Average Surface Roughness (RMS) values and the average surface grain size are

shown in Table 2. These results are agreement with Mazón-Montijo, et al, 2010 [29]

. The grain

size of the film was determined using the AFM, the average grain size increases as increasing

Ta because the increasing Ta can cause recrystallization in grains, leading to a reorientation of

the film and a significant increase in average grain size. Consequently, the surface roughness

increases as increase the grain size.


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Table 2. Crystallite size, roughness average, and Ta of CdS.

Ta (K) Grain size average (nm) Root mean

square (nm)

Roughness

average (nm) Peak-peak (nm)

300 32.5 1.51 1.30 11.5

400 46.7 1.91 1.93 13.4

500 61.1 2.42 2.32 15.3

600 86.2 3.11 2.71 18.6

The optical transmittance spectra of as-deposited and annealed CdS was recorded as a

function of wavelength as shown in Fig 3.

.

Fig. 3. Transmittance variation with the wavelength

The transmittance spectra of CdS exhibited a sharp fall at the fundamental absorption

edge of approx. 500 nm. Fig. 4

Gradual enhancement in absorbance was noted with an increase in annealing

temperature. The annealed samples show a slight shift in the absorbance toward higher

wavelength with the increase of annealing temperature. The band gaps of the films were

calculated using Tauc equation by plotting the relations of (αhυ)1/2

versus incident photon

energy (hυ) as shown in Fig. 5.

0

20

40

60

80

100

120

200 300 400 500 600 700 800 900

a: RT

b: Ta=400 K

c: Ta=500 K

d: Ta=600 K

abcd

λ nm

T%


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Fig. 4. Absorbance with the wavelength

Fig. 5. (hυ)

2 vers. hυ

The gap energy was obtained by extrapolating the straight line portion of the graph to

zero absorption coefficients. The intercept on the energy axis gives the value of gap energy.

The plot indicates the transition is an allowed direct type. The as-deposited sample showed

direct band gap of 2.44 eV, which was found to reduce to 2.27 eV with annealing.

0

20

40

60

80

100

200 400 600 800 1000λ nm

A%

dc

b a

a: RT

b: Ta=400 K

c: Ta=500 K

d: Ta=600 K

0.0E+00

2.0E+09

4.0E+09

6.0E+09

8.0E+09

1.0E+10

1.2E+10

1.5 2 2.5 3

d

a

b

c

a: RT

b: Ta=400 K

c: Ta=500 K

d: Ta=600 K

hυ (eV)

(αhυ

)^2 (

eV

.Cm

)^-2


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The obtained values were found to be comparable with the previous reports [25–27]

. The

sample annealed at 600 °C showed minimum band gap (2.27 eV). This deviation of band gap

from 2.44 eV to ...2 eV can be attributed to the change in crystallite size as a result of

controlled annealing [28]

. The observed improvement in the crystallites of samples can be

correlated with the optical study, reflecting a red shift in the optical band gap of the material

which is justified by increased crystallite size and crystalline quality. The Different values of

the refractive index against incident photon energy (hυ) for all samples which prepared at R.T

and annealed is shown in Fig. 6, the refractive index for all samples is about 2.18.

Fig. 6. n vers. hυ

The demeanor of the extinction coefficient k of CdS for different annealing

temperatures is shown in Fig. 7. It makes us realize easily that the extinction coefficient, in

general, increases with increasing of annealing temperature (Ta).

The variation of the εr and εi versus photon energy (hυ) for CdS films for different

annealing temperature shown in Figs. (8, 9). The behavior of εr is similar to that of the (n)

because of the smaller value of k. compared with n

. , while εi is mainly depended on the k

values.

The variation of the energy gap and the optical parameter with annealing temperature

are given in Table 3. These results are agreement with Mariappan, et.al, 2012 [28]

.

0

0.5

1

1.5

2

2.5

1 1.5 2 2.5 3 3.5 4

hυ (eV)

a: RT

b: Ta=400 K

c: Ta=500 K

d: Ta=600 K

n

dcba


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Fig. 7. k vers. hυ

Fig. 8. ɛr vers. hυ

0

0.05

0.1

0.15

0.2

0.25

1.5 1.7 1.9 2.1 2.3 2.5 2.7 2.9

hυ (eV)

kd c b aa: RT

b: Ta=400 K

c: Ta=500 K

d: Ta=600 K

0

0.5

1

1.5

2

2.5

3

3.5

4

4.5

5

1 1.5 2 2.5 3 3.5 4

dc

ba

hυ (eV)

ɛ r

a: RT

b: Ta=400 K

c: Ta=500 K

d: Ta=600 K


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Fig. 9. ɛi vers. hυ

Table 3. The dependence of the band gap, extinction coefficient, refractive

Index, and the real and imaginary parts of dielectric constant

Ta (K) Eg (eV) n k εr εi

300 2.44 2.18 0.17 449 0.38

400 2.35 2.18 0.15 4.48 0. 41

500 2.32 2.18 0.11 4.49 0.65

600 2.27 2.18 0.08 4.50 0.71

4. CONCLUSIONS

CdS were prepared using spray pyrolysis and deposited on the slide at 350 °C. The

corresponding characteristics of the CdS as a function of annealing temperature were

reported. X-ray results show that the structure of CdS is polycrystalline with a hexagonal

quartzite structure. The refractive index is about 2.18. The grain size increased with

increasing annealing temperature. The linear dependence of (αhν)2 to hν indicates that CdS at

all different annealing temperature are direct transition type semiconductors. It concluded that

the decreases in the optical band gap of the films with increasing annealing temperature.

0

0.1

0.2

0.3

0.4

0.5

0.6

0.7

0.8

1 1.5 2 2.5 3 3.5 4hυ (eV)

ɛi

a: RT

b: Ta=400 K

c: Ta=500 K

d: Ta=600 K

dcba


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Acknowledgement

The authors acknowledge the financial support of the Kufa and Baghdad Universities, Iraq. The authors are

grateful to Dr. Basim A. Almayahi, Department of Environment, College of Science, University of Kufa

([email protected]) for assisting us throughout conducting the present research.

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( Received 28 September 2017; accepted 16 October 2017 )

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Structural and optical properties of nanocrystalline CdS films … · 2017. 10. 16. · CdS films prepared by spray pyrolysis Radhyah M. S. Aljarrah, Adnan H. Aljobory* Department