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AUTHOR'S
PROOF

Article Title

Structural and Optical Characterization of Chemically Deposited

PbS Thin Films

Article Sub-Title

Article Copyright - Springer Science+Business Media Dordrecht 2016

(This w ill be the copyright line in the final PDF)
Year

Journal Name

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Family Name

Particle

Given Name

Suffix

Fouda
A. N.

Organization

Suez Canal University

Division

Physics Department, Faculty of Science

Address

41522, Ismailia, Egypt

12

Organization

University of Hail

13

Division

Recruitment Department

14

Address

Hail 2440, KSA, Hail, Saudi Arabia

15

e-mail

alynabieh@yahoo.com

16

Family Name

Marzook

17

Particle

18

Given Name

19

Suffix

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11

20

Corresponding
Author

Author

M.

Organization

Suez University

21

Division

22

Address

Basic Science Department, Faculty of Petroleum

and Mining Engineering
43721, Suez, Egypt

23

e-mail

None

24

Family Name

Abd El-Khalek

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Given Name

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28

Author

H. M.

Suffix
Organization

Suez Canal University

29

Division

Physics Department, Faculty of Science

30

Address

41522, Ismailia, Egypt

31

e-mail

None

32

Family Name

Ahmed

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34
35

Author

Particle
Given Name
Suffix

S.

AUTHOR'S PROOF
36

Organization

Suez University

37

Division

38

Address

Basic Science Department, Faculty of Petroleum

and Mining Engineering
43721, Suez, Egypt

39

e-mail

None

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Family Name

Eid

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Given Name

43
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Author

E. A.

Suffix
Organization

Higher Technological Institute

45

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Department of Basic Science

46

Address

10th of Ramadan City, Ramadan, Egypt

47

e-mail

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Family Name

El Basaty

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50

Given Name

51

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52

Author

A. B.

Organization

Helwan University

53

Division

54

Address

Basic Science Department, Faculty of Industrial

Education
11813, Cairo, Egypt

55

e-mail

None

56

Received

19 May 2015

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Schedule

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Revised
Accepted

28 December 2015

59

Abstract

PbS thin films were deposited on glass substrates by chemical bath

deposition method. The effect of varying the film thickness on the
structural and optical properties has been investigated. XRD
analysis reveals the crystallinity of the deposited PbS films with
(200) preferred crystal orientation. Increasing the film thickness
enhances the crystallinity of the films as well as decreases the strain
and dislocation density. The surface morphology features were
dramatically changed from small spherical grains to beads like
shape. The absence of impurities in the deposited films were
confirmed by energy dispersive x-ray spectrometry (EDX)
measurements. The optical constants of the deposited films were
calculated and a little decrease in the band gap energy was
observed with increasing the film thickness.

60

Keywords
separated by ' - '

PbS films - Chemical bath deposition - Surface morphology - XRD

61

Foot note
information

JrnlID 12633 ArtID 9399 Proof#1 - 05/01/2016

AUTHOR'S PROOF
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DOI 10.1007/s12633-015-9399-z

ORIGINAL PAPER

2
3

Structural and Optical Characterization of Chemically

Deposited PbS Thin Films

6
7

Received: 19 May 2015 / Accepted: 28 December 2015

Springer Science+Business Media Dordrecht 2016

Abstract PbS thin films were deposited on glass substrates by

chemical bath deposition method. The effect of varying the
film thickness on the structural and optical properties has
been investigated. XRD analysis reveals the crystallinity of
the deposited PbS films with (200) preferred crystal orientation. Increasing the film thickness enhances the crystallinity
of the films as well as decreases the strain and dislocation
density. The surface morphology features were dramatically changed from small spherical grains to beads like
shape. The absence of impurities in the deposited films were
confirmed by energy dispersive x-ray spectrometry (EDX)
measurements. The optical constants of the deposited films
were calculated and a little decrease in the band gap energy
was observed with increasing the film thickness.

10
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23

Keywords PbS films Chemical bath deposition Surface

morphology XRD

 A. N. Fouda

alynabieh@yahoo.com

Q1
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1 Introduction

24

PbS is one of the most important IV-VI semiconductors with

narrow band gap of 0.41 eV at 300 K [1], and sufficiently
large Bohr radius of 18 nm [2]. This provides strong quantum confinement of holes and electrons, regulating the band
gap value by controlling the crystallite size according to the
effective mass model [3]. PbS thin films have been a subject of extensive research due to their wide applications in
gas sensors [4], infrared radiation detectors [5, 6], optoelectronics, solar cells, diode laser, etc [7, 8]. PbS thin films
are p-type semiconductors [9], and their direct band gap are
around 2.2 eV [9]. For these reasons, many research groups
have shown a great interest in the study and enhancement
of this material by various depositional processes. PbS thin
films can be deposited by different chemical and physical methods, such as vacuum evaporation [10], successive
ionic layer adsorption and reaction (SILAR) [11], electrodeposition [12], chemical bath deposition (CBD) [13, 14],
etc. Among these, CBD is the most simple, low temperature
requirement, low-cost, able to deposit thin films on different
types of substrates, and convenient for large area deposition.
CBD method is based on successive absorption and reaction
of species on the substrate surface from aqueous solution
containing Pb2+ and S2. Film growth takes place by cluster mechanism or ion-by-ion. In this method, we can deposit
a good adhesive films with different optical and structural
properties by optimizing the bath temperature [15], reactant
pH [16], reagent concentration [17], and deposition time
[18]. A comparative study has been performed on properties of PbS thin films grown by CBD, TEA was used as the
complexing agent in one of the baths, and PbS films were
prepared without Triethanolamine (TEA) [19]. Ubale et al.

25

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A. N. Fouda1,2 M. Marzook3 H. M. Abd El-Khalek1 S. Ahmed3 E. A. Eid4

A. B. El Basaty5

Physics Department, Faculty of Science, Suez Canal

University, 41522 Ismailia, Egypt
Recruitment Department, University of Hail,
Hail 2440, KSA Hail Saudi Arabia
Basic Science Department, Faculty of Petroleum and Mining
Engineering, Suez University, 43721 Suez, Egypt
Department of Basic Science, Higher Technological Institute,
10th of Ramadan City, Ramadan Egypt
Basic Science Department, Faculty of Industrial Education,
Helwan University, 11813 Cairo, Egypt

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presented the synthesis of nanocrystalline PbS thin films

using CBD method where concentration of Pb2+ and S2
ions, temperature and pH were optimized to obtain good
quality of PbS thin films on glass [9].
In this work, PbS thin films were deposited by CBD with
different film thicknesses at room temperature. The structural and optical properties of the prepared films were studied by using X-ray diffraction (XRD), scanning electron
microscopy (SEM), and UV-VIS-NIR spectrophotometer.

2 Experimental
Lead sulfide thin films have been synthesized on glass substrates using CBD method. The glass substrate was cleaned
using ultrasonic baths of acetone, dichloromethanol and
methanol. Then, we rinsed it with deionized water. CBD
solution was prepared by sequential addition of 2.5 ml (0.5
M) of lead acetate Pb(CH3 COO)2 , 2.5 ml (2 M) of sodium
hydroxide (NaOH), 1 ml (1 M) of triethanolamine (TEA)
C6 H15 NO3 , and 3 ml (1 M) of thiourea CH4 N2 S. At room
temperature (25 C), deionized water was added until the
total volume of the solution reached 70 ml, and the pH was
11. The cleaned substrates were vertically immersed in 100
ml beaker, containing the CBD solution. The reactions of
the PbS formation on the glass substrate are given as:
[P b(CH3 COO)2 .3H2 O + 2NaOH ] P b(OH )2

Q3
79

+2Na(CH3 COO) + 3H2 O

(1)

:OH

SC(NH2 )2 + 2H2 O H2 S(g) + CO2(g)

:OH

+2NH3(g) S 2 + H2 O

Fig. 1 Schematic diagram

describe the procedure PbS
films preparation

2P b(OH)2+ 2[C6 H15 N O 3 ]n 2[P b(T EA)n ]+ 2H2 O+O2 (3)

80

[P b(T EA)n ] P b

2+

(2)

2.5 ml (0.5 M) of
lead acetate

+ n (T EA)

(4)
81

P b2+ + S 2 P bS

(5)

The samples labeled S1, S2, S3 and S4 for deposition

times of 1h, 2h, 3h, and 4h respectively. The deposited
films were cleaned in an ultrasonic bath with deionized
water. The obtained films were homogeneous without color
degradation, and good adherent to the substrate. The color
of the films was light brown for S1 and going darker with
increasing the deposition time.
The structure and the average particle size of the
deposited lead sulfide films were determined by X-ray
diffraction (XRD) using a P-analytical XPERT PRO Materials Research Diffractometer. Data were collected in the
2/ geometry and were recorded in the range of 20 70
at 45 kV and 40 mA
using Cu K radiation ( = 1.54 A)
(Fig. 1).
The surface morphology of the PbS films was studied using a FEI QUANTA FEG 250 scanning electron
microscopy (SEM). Film thickness was measured using
interference microscopy and further confirmation was performed from side-view of SEM images as shown in Fig. 4.
The thicknesses of S1, S2, S3, and S4 were 47, 83, 105, and
133 nm respectively.
The elemental composition of the films was determined
by the energy-dispersive X-ray analysis (EDX) using a FEI
QUANTA FEG 250. The measurements were extended to
optical characterizations in the wavelength range from 380

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2.5 ml (2 M) of
sodium hydroxide

1 ml (1 M) of triethanolamine

3 ml (1 M) of
thiourea

Water
added

After 1 hour
After 2 hours

4 glass plates
immersed

After 4 hours
After 3 hours

S4

S1
S2

S3

82
83
84
85
86
87
88
89
90
91
92
93
94
95
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101
102
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105
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(311)

(222)

(220)

(200)

INTENSITY (arb. units)

(111)

Silicon

temperature are shown in Fig. 2. All the films are

polycrystalline with (200) preferred crystal orientation. The characteristic reflection peaks of PbS are observed
at 25.8 , 29.9 , 42.9 , and 50.9 for (111), (200), (220),
and (311) planes, respectively. An increment in the peak
intensity can be observed with increasing the film thickness
for S1, S2, and S3. In the case of S4, irregular trend was
observed and this can be attributed to the surface topography of the sample as shown in Fig. 3. Similar behavior was
reported by other groups [17].
Generally with increasing the film thickness, an enhancement in the crystallinity was established. The crystallite size was calculated using the well-known Scherrers
formula:

S4

S3

S2

S1

20

30

40

50

60

D=

to 1200 nm using a UV/VIS/NIR double beam spectrophotometer (JASCO V-570).

3 Results and Discussion

110

Representative XRD of PbS films with different film

thickness which deposited on glass substrates at room

111

Fig. 3 SEM photographs of the

S1, S2, S3, and S4

115
116
117
118
119
120
121
122
123
124
125

(6)

Where is the wavelength (1.5406 A),

is the
full width at half maximum of the peak (in radians),
and is the Braggs diffraction angle. PbS films exhibited a remarkable increase in the crystallite size
with increasing the film thickness and it can be attributed to
the coalescence between neighboring islands during compacted deposition and atomic mass transport. Moreover, the

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0.9
cos

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Fig. 2 X-ray diffraction patterns for the S1, S2, S3, and S4

108

114

70

2 (degree)

107

112
113

(S1)

(S3)

(S2)

(S4)

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129
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Sample

(h k l)

d(A)

a(A)

(PDF: 05-0592)

(111)
(200)
(220)
(311)

3.427
2.968
2.099
1.790

5.936
5.936
5.936
5.936

(111)
(200)
(220)
(311)

3.449
2.977
2.102
1.796

5.9746
5.9536
5.9465
5.9559

9.5

(111)
(200)
(220)
(311)

3.448
2.977
2.104
1.791

5.972
5.954
5.951
5.939

9.9

(111)
(200)
(220)
(311)

3.441
2.976
2.105
1.794

5.960
5.952
5.953
5.948

11.6

(111)
(200)
(220)
(311)

3.431
2.963
2.098
1.789

5.942
5.927
5.933
5.934

12.7

S1

S2

S3

132
133

dislocation density can be derived from the crystallite size

using the formula [20]:
=

134
135

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S4

1
D2

(7)

The lattice strain () of S1, S2, S3, and S4 was calculated

from the relation [19]:
cos
=
4

Fig. 4 Cross-sectional scanning

electron microscopy (SEM) of
S3, and S4

(8)

D (nm)

1020 (lines/cm2 )

103

t1.1
t1.2
t1.3
t1.4
t1.5

1.108

3.78

t1.6
t1.7
t1.8
t1.9

1.02

3.63

t1.10
t1.11
t1.12
t1.13

0.743

3.12

t1.14
t1.15

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Table 1 (hkl), d, a, crystallite

size , Dislocation density, and
lattice strain values of the PbS
films

Q6

0.62

t1.16
t1.17

2.84

t1.18
t1.19
t1.20
t1.21

The calculations were extended to the micro strain within

the samples to demonstrate the effect of dislocation density
on the film quality. The decrease in the strain with increasing the film thickness reflects the relaxation of thicker
films [21].
The lattice parameter (a) of S1, S2, S3, and S4 was calculated for the cubic structure of PbS with inter-planer spacing
(d) using
1
h2 + k 2 + l 2
=
d2
a2

(9)

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EDX (S1)

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EDX (S2)

respectively, which are comparable to the bulk lattice

parameter (a = 5.936) [22]. The dependence of a, d, and
dislocation density on the film thickness are summarized in
Table 1.
Figure 4 shows cross sectional view of samples S3, and
S4 which used to confirm the previously measured thickness by interference microscope. The surface morphology
of the deposited films are shown in Fig. 3. Isolated islands
with intermediate spaces can be seen. For S1, regularly
well-organized small grains can be observed. With increasing the film thickness, beads like shape and agglomeration
of grains is distinguished. S2, S3 and S4 images evidence
that elongated grains are randomly oriented and coalescence
at different regions. With increasing the film thickness the
surface roughness increases due to the growth of isolated
islands together and agglomeration effect was observed
beside elongation of needle shapes.
Compositional analysis was determined by EDX (energy
dispersive spectrometry) measurements. Figure 5 shows the
EDX patterns of S1, S2, S3, and S4. The patterns display several mean peaks at different energy values, which
correspond to the Pb and S elements. It is observed that the
atomic or weight concentration of each element varies with
increasing the film thickness which can be attributed to the
rate of chemical reaction. It was clear that the composition
of the deposited films contains the elements of Pb and S
beside the peaks of glass. It is well known that the composition of glass consists of 75 % SiO2 , sodium oxide Na2 O,
sodium carbonate Na2 CO3 , calcium oxide CaO, and several minor additives [23]. The transmittance and reflectance
spectra recorded for S1, S2, S3, and S4 are shown in
Fig. 6. The drop in the reflectance around the band edge
is related to the increase in transmission, and the observed
interference behavior is related to the film thickness and surface morphology. The reflectance decreases with increasing
the film thickness in the spectra range from 400 to 1100
nm which can be attributed to the morphological features. The grain size increases with increasing the film
thickness [20].
The transmission edge is shifted toward longer wavelength with increasing the film thickness. The band edge
shift is related to the decrease in the direct band gap
energy. The absorption coefficient was calculated using the
following equation [23]:

EDX (S3)

EDX (S4)

 
1
1
= ln
t
T
Fig. 5 EDX measurements for S1, S2, S3, and S4

144

For (200) plane, the calculated lattice parameters are

5.953, 5.954, 5.952, and 5.927 for S1 , S2, S3, and S4

146
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180
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182
183
184
185
186
187
188

(10)

Where t is the film thickness and T is the transmittance. The

band gap energy of S1, S2, S3, and S4 were calculated using
the Tauc equation [24, 25]:
h = A(h Eg )1/2

145

(11)

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Fig. 6 Variation of
transmittance and reflectance
with wavelength for S1, S2, S3,
and S4

100

60

1
2
3
4

80

50
40

R%

T%

60
40

30
20

20
0

1
2
3
4

10
400

600

800

1000

1200

400

600

[nm]

196
197
198
199
200
201
202
203
204
205
206

16

2.0x10

16

1.8x10

16

1.6x10

S(1)
S(2)
S(3)
S(4)

16

1.4x10

1200

gives the relation between bulk band gap and nano-structure

band gap:


h2 2 1
1
1.78e2
Eg (nano) = Eg (bulk) +
+

mh
r
2r 2 me
(12)

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195

1000

Where me and mh are the effective masses of the electron in the conduction band and the hole in the valence
band, respectively; r is the radius of the particle; and
is the dielectric constant of PbS (value of 17.3). Due
to the quantum localization (i.e. the kinetic energy) of
the second term, Eg is shifted to higher energies. The
third term represents the screened Coulomb interaction
between holes and electrons, which shifts Eg to lower
energies [27, 28].
The refractive index (n) is related to the optical reflectance (R), by the following relation [29]:

1
2
4R
1+R
2
+
n=
k
(13)
2
1R
(1 R)

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194

Where (k) is the extinction coefficient which is related to

the absorption coefficient () and the wavelength () by:

16

193

Where A is constant, h is Plancks constant, is the frequency of photon, and Eg is the energy gap. The variation
of (h)2 versus h (photon energy) is shown in Fig. 7. The
extrapolation of the curve is used to calculate the energy
gap [26]. As the thickness decreases, the calculated band
gap energy for the prepared samples ranges from 2.34 to
2.75 eV as tabulated in Table 2. The energy gap decreases
with increasing the film thickness. This is related to the
increment in the crystallite size with increasing the film
thickness. Although, the reported band gap energy of bulk
PbS ranges from 0.4 to 0.6 eV. The obtained higher values can be attributed to the quantum confinement effect.
After certain limiting size of particle size which associated
with the exciton Bohr radius, the space between band levels is changed. The Brus Model of nano-structure band gap

( h )

192

800
[nm]

k=

1.2x10

16

1.0x10

207
208

209
210
211
212
213
214
215
216
217
218
219

220
221

(14)

15

8.0x10

Table 2 Energy gap values of S1, S2, S3, and S4

15

6.0x10

15

4.0x10

t2.1

Sample

Thickness (nm)

Eg (eV)

t2.2

S1
S2
S3
S4

47
83
105
133

2.75
2.61
2.44
2.34

t2.3

15

2.0x10

0.0

1.5

2.0

2.5

3.0

h [eV]
Fig. 7 Plot of (hv)2 vs. hv of S1, S2, S3, and S4

3.5

4.0

t2.4
t2.5
t2.6

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8

1.4

6
5
4
3
2

1
2
3
4

1
400

600

800

226
227
228
229
230
231
232
233
234
235
236
237
238
239

Fig. 9 Variation of the real (1 )

and imaginary (2 ) parts of
dielectric constant with
wavelength for S1, S2, S3, and
S4

0.6
0.4
0.2
400

600

800

1000

1200

[nm]

increasing the film thickness, due to the increase of the

absorption with increasing the film thickness, which agrees
with previous reports [30, 31]. The spectra of extinction
coefficient for different thickness of S1, S2, S3, and S4
show a dominant peak around 380416 nm as shown in
Fig. 8b.
The real (1 ) and imaginary 2 ) parts of the dielectric
constant of the prepared films can be calculated from [32]:
1 = n2 k 2

2 = 2nk

60

8
1
2
3
4

50

1
2
3
4

7
6

40

30

4
3

20

2
10
0

1
400

600

800
[nm]

1000

1200

400

600

240
241
242
243
244
245
246
247

(15)

The variation of these two parameters with wavelength is

shown in Fig. 9. The values of the real part (1 ) increases
with wavelength while the imaginary part (2 ) of the dielectric constant decreases with wavelength of all samples
except S1. Since the values of the refractive index is larger
than k values, the behavior of 1 is similar to n. The variation
of absorption coefficient has a direct effect on the values
of 2 .

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0.8

0.0

1200

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1.0

[nm]

The variation of refractive index (n) with is shown in

Fig. 8a. The retardation of light in the film is very high in the
NIR region and decays to relatively low rate in the visible
region. The n value of S1, S2, S3, and S4 extended from
2.1 to 6.8. The change of refractive index with wavelength
open the door to the usage in optoelectronic devices, since
the wave propagation is strongly influenced by the distribution of the refractive index. It is clear from the Figure that
the refractive index increases as the thickness decreases in
the visible region and it decreases as the thickness decreases
in the IR region except the smaller film thickness. The
scattering of light within the smaller thickness exhibited
different trend because of its smaller and uniform grain
distribution.
The extinction coefficient as a function of the incident wavelength is shown in Fig. 8b. From the figure, we
can notice that the extinction coefficient is related to the
absorption of light within the films. k values decrease with

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1000

1
2
3
4

1.2

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extinction coefficient ( )

refractive index (n)

Fig. 8 Variation of refractive

index (n) and extinction
coefficient (k) with wavelength
for S1, S2, S3, and S4

800
[nm]

1000

1200

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AUTHOR'S PROOF

Silicon

4 Conclusions

257

268

The effect of varying the film thickness on the structural, surface morphology and optical properties of PbS
films was investigated. The deposited films by chemical
bath deposition were polycrystalline with (200) preferred
crystal orientation. The thicker films exhibited bigger crystalline size which influences on the optical constants. The
purity of the films were confirmed by EDX measurements
and the surface morphology is changed from small spherical shaped grains to bigger agglomerated rod like grains
with increasing the film thickness. The change of refractive
index with wavelength reflects the possibility of usage in
optoelectronic devices.

269

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