This paper reports on the deposition and surface properties of the pure and doped zinc oxide layers
produced by spin coating route. Pure and metallic (Al, Sn, Cd, Co) doped ZnO films are characterized by
mean of atomic force microscopy (AFM). Based on atomic force microscope observation, some parameters
such as grain size, height, orientation of angle and histogram are determined. The AFM scanned 2D and
3D-views permit us to discover the roughness, the average height and the skewness of clusters or grains

Avila-Garcia, A.

Benhaliliba, M.

Tiburcio-Silver, A.

English

SocioEconomic Challenges Journal (Sumy State University)

JOURNAL OF NANO- AND ELECTRONIC PHYSICS ЖУРНАЛ НАНО- ТА ЕЛЕКТРОННОЇ ФІЗИКИ 
Vol. 7 No 4, 04012(7pp) (2015) Том 7 № 4, 04012(7cc) (2015) 
 
 
2077-6772/2015/7(4)04012(7) 04012-1  2015 Sumy State University 
AFM Calculated Parameters of Morphology Investigation of Spin Coated MZO  
(M  Al, Sn, Cd, Co) Layers 
 
M. Benhaliliba1,*, A. Tiburcio-Silver2, A. Avila-Garcia3 
 
1 Department of Material Technology, Physics Faculty, USTOMB University, BP1505 Oran, Algeria 
2 ITT-DIE, Apdo, Postal 20, Metepec 3, 52176 Estado de Mexico, Mexico 
3 Cinvestav-IPN, Dept. Ingeniería Eléctrica-SEES, Apdo. Postal 14-740, 07000 México, D.F., Mexico 
 
 (Received 17 August 2015; published online 10 December 2015) 
 
This paper reports on the deposition and surface  properties of the pure and doped zinc oxide layers 
produced by spin coating route. Pure and metallic (Al, Sn, Cd, Co) doped ZnO films are characterized by 
mean of atomic force microscopy (AFM). Based on atomic force microscope observation, some parameters 
such as grain size, height, orientation of angle and histogram are determined. The AFM scanned 2D and 
3D-views permit us to discover the roughness, the average height and the skewness of clusters or grains. 
 
Keywords: Spin coating, ZnO layer, Metallic dopant, Atomic force microscope, Grain size, Roughness, 
Histogram. 
 
 PACS numbers: 68.37.Ps, 68.35.Ct, 81.05.Cy 
 
                                                                
* mbenhaliliba@gmail.com 
1. INTRODUCTION 
 
Nanostructures of pure and metallic doped ZnO are 
largely investigated in the search for improved properties 
and new applications due to its remarkable optical and 
electric properties. Growth of such layers is made by many 
processes like spray pyrolysis, spin and dip coating [1-6]. 
In this research, MZO (M  Al, Sn, Cd, Co) layers are 
fabricated by a facile and low cost spin coating technique. 
AFM details of morphology investigation of MZO (M  Al, 
Sn, Cd, Co) are explored, emphasized and calculated by 
the mean of 2D, 3D and histogram curves. In order to 
improve quality of topography of such nanostructures and 
their different properties and their use in micro and nano-
electronic we fabricate such films. 
 
2. PREPARATION AND ANALYSIS OF THE 
LAYERS  
 
The ZnO layers have been grown by sol gel spin coat-
ing route onto glass slides 76  26 mm substrate at speed 
of 1000 rpm. 0.5 Molar of dihydrated zinc acetate  
(Zn (CH3COO)2.2(H2O)), (99.5 %) supplied by Carlo Erba 
reagents, is dissolved in 10 ml of 2-Methoxyethanol stirred 
at 60 °C for 10 mn and then 0.3 ml of the mono-
ethanolamine (MEA) as stabilizer  is added drop by drop, 
the clear solution is then obtained, the stirring continued 
for 60 min. The surface morphology of samples is analyzed 
by atomic force microscope (AFM) observation using a 
Quesant Model 250 system having an (80 m  80 m) 
head, in the wave mode in air. For the (3 m  3 m) 
square images the resolution is (300  300) pixels at a 
fixed scan rate of 2 Hz. All analyses are performed with 
the WSXM system software. 
 
3. DATA AND PARAMETERS DICUSSION 
 
The root mean square (RMS) is given by [7], 
 
 
1
( )²m iRms Z Z
N
   (1) 
 
 
Where N is the number of deviations, Zi is the height 
reference and Zm is the profile value. As tabulated be-
low (Table 1), grain size, height, orientation angle and 
histogram parameters are determined using AFM ob-
servation and its suitable software. These analyses 
revealed the presence of assembled grains which have 
several orientations, shapes, roughnesses and sizes. 
The statistical distribution or height histogram showed 
a difference in intensity of bars (%), around 1600 for 
the ZnO case and 350 for the Cd (3 %) doped layer case. 
The ZnO layer presents an average height of 93 nm a 
roughness (RMS) deviation of 56 nm as shown in Fig. 1 
(height histogram). While the Al doped ZnO exhibits a 
height of 198.9 and 379 nm and RMS of 94 and 237 nm for 
2 % and 3 % Al doping level respectively. Doped by cad-
mium, the layers present a height of 198 and 436 nm and 
RMS of 76 and 229 nm respectively for 2 and 3 % Cd dop-
ing level into solution as indicated in Table 1. The scanned 
AFM pictures showed a large amount of grain agglomera-
tion that looked like assembled nanotips or nanocolumns 
with broadened heads and few voids as shown in Fig. 1. In 
3D-shape, we observe the highest grain reached a value of 
482 nm. The hollow ZnO nanocolumns have been fabri-
cated by electrochemical deposition as reported by Cem-
brero [8]. The Figure 2 demonstrates the images of AFM 
analysis, 2D view and the histogram as function of size 
along x-axis. 3D-views and height histogram distribution 
of 2 % Al doped ZnO layers produced by spin coating tech-
nique are displayed in inset of the Figure 2. 
The analyzed grains are assigned by yellow arrows in 
2D and 3D images. The height histogram seems to be 
composed of many profiles where no symmetry occurs 
except the case of 2 and 3 % Sn and 2 % Cd doped ZnO 
films present a shape close to Gaussian distribution where 
a high symmetry of area height distribution is demon-
strated. This result is confirmed by the homogeneity sur-
face of sample which is easily seen in 3D-view (see Fig-
ures 4-6). It is reported in literature that AFM image 
shows hexagonally faceted columnar grains that dominate 
the surface morphology of (Al, B) co-doped ZnO by sol-gel 
process using spin coating procedure [9]. 
 M. BENHALILIBA, A. TIBURCIO-SILVER, A. AVIRA-GARCIA J. NANO- ELECTRON. PHYS. 7, 04012 (2015) 
 
 
04012-2 
 
 
 
 
 
 
 
 
 
 
 
 
 
 
 
 
 
 
Fig. 1 – Images of AFM analysis, 2D view and the histogram 
as function of size along x-axis (grains A and B) (I, II). 3D-
views and height histogram distribution of pure ZnO layers 
(III, IV) produced by spin coating technique. The analyzed 
grains are assigned by yellow arrows in 2D and 3D images 
 
 
 
 AFM CALCULATED PARAMETERS OF MORPHOLOGY INVESTIGATION… J. NANO- ELECTRON. PHYS. 7, 04012 (2015) 
 
 
04012-3 
Table 1 – Description of the topography parameters of pure and M-doped ZnO produced by spin coating process  @ 1000 rpm 
 
№ Material Grain size 
(m) 
Height z 
(nm) 
Orientation 
angle (°) 
Histogram parameters 
Average height (nm) RMS deviation (nm) 
1 Undoped ZnO/Glass (grain A) 1.16 7.17 89.6 93.10 59 
2 Undoped ZnO/Glass (grain B) 0.84 17.52 89.2 93.1 59 
3 2 % Al doped ZnO / Glass 0.51 28.6 86.8 198.8 94.17 
4 3 % Al doped ZnO / Glass 0.54 6.38 89.8 378.7 237.2 
5 2 % Sn doped ZnO / Glass 0.63 36.51 86.7 85.25 28.65 
6 3 % Sn doped ZnO / Glass 0.51 0.50 89.9 124.3 41.9 
7 2 % Cd doped ZnO / Glass 1.44 38.7 88.5 197.7 75.9 
8 3 % Cd doped ZnO / Glas 1.35 42.3 88.2 435.7 228.6 
9 Co doped ZnO / ITO 0.30 79.3 75.3 362 167.8 
 
 
 
Fig. 2 – Images of AFM analysis, 2D view and the histogram 
as function of size along x-axis. 3D-views and height histo-
gram distribution of 2 % Al doped ZnO layers produced by 
spin coating technique. The analyzed grains are assigned by 
yellow arrows in 2D and 3D images 
 
 
 
 
 
 
 
 
Fig. 3 – Images of AFM analysis, 2D view and the histogram as 
function of size along x-axis. 3D-views and height histogram 
distribution of 3 % Al doped ZnO layers produced by spin coating 
technique. The analyzed grains are assigned by yellow arrows in 
2D and 3D images 
 
 
 
 M. BENHALILIBA, A. TIBURCIO-SILVER, A. AVIRA-GARCIA J. NANO- ELECTRON. PHYS. 7, 04012 (2015) 
 
 
04012-4 
 
 
 
 
 
 
Fig. 4 – AFM analysis pictures, 2D view and the histogram as 
function of size along x-axis. 3D-views and height histogram 
distribution of 2 % Sn doped ZnO layers produced by spin 
coating technique. The analyzed grains are assigned by yellow 
arrows in 2D and 3D images 
 
 
 
 
 
 
 
 
Fig. 5 – AFM analysis pictures, 2D view and the histogram as 
function of size along x-axis. 3D-views and height histogram 
distribution of 3 % Sn doped ZnO layers produced by spin 
coating technique. The analyzed grains are assigned by yellow 
arrows in 2D and 3D images 
 
 
 AFM CALCULATED PARAMETERS OF MORPHOLOGY INVESTIGATION… J. NANO- ELECTRON. PHYS. 7, 04012 (2015) 
 
 
04012-5 
 
 
 
 
 
 
Fig. 6 – The pictures of AFM analysis, 2D view and the histo-
gram as function of size along x-axis. 3D-views and height 
histogram distribution of 2 % Cd doped ZnO layers produced 
by spin coating technique. The analyzed grains are assigned 
by yellow arrows in 2D and 3D images 
 
The surface morphology of the ZnO film is practical-
ly smooth, with uniform grain distribution and the 
surface roughness was found to be 17 nm as cited by 
Sharma [10]. All our samples are roughly in well 
agreement with those found in literature. 
The surface of as-grown ZnO layers, produced by 
spin coating technique, is composed by some non uni-
form domains. A topography of films was columnar as 
Smirnov mentioned in his work [14]. 
Furthermore, AFM images indicate that the ZnO 
films, deposited by sol gel spin coating, are formed from 
the nanoparticles as cited in literature [11] which cor-
roborate with our results. Produced by a sol gel spin 
coating method @ 3000 rpm, the ZnO layers demon-
strate the presence of a porous structure and the film 
surface for as-grown sample is very coarse with the 
root mean square (RMS) of 22.42 nm as Srinivasan 
reported [12] while our layers are more rough 
RMS  40 nm. This fact might due to the minor speed ( 
 
 
 
 
 
 
 
 
Fig. 7 – The images of AFM analysis, 2D view and the histo-
gram as function of size along x-axis. 3D-views and height 
histogram distribution of 3 % Cd doped ZnO layers produced 
by spin coating technique. The analyzed grains are assigned 
by yellow arrows in 2D and 3D images 
 
1000 rpm) of spin coating process used for the growth 
of our films. Moreover, the columnar character of the 
grains of pure and Fe-doped ZnO layer, prepared by 
spin coating at 3000 rpm, indicates the preferentially  
 M. BENHALILIBA, A. TIBURCIO-SILVER, A. AVIRA-GARCIA J. NANO- ELECTRON. PHYS. 7, 04012 (2015) 
 
 
04012-6 
 
 
 
 
 
 
 
Fig. 8 – The AFM analysis pictures, 2D view and the histo-
gram as function of size along x-axis. 3D-views and height 
histogram distribution of Co doped ZnO layers produced by 
spin coating technique. The analyzed grains are assigned by 
yellow arrows in 2D and 3D images 
 
growth along the z-axis direction perpendicular to the 
substrate surface as revealed by Rambu et al. [13]. 
The size of selected grains accurately showed by ar-
row in 2 and 3D views are determined by two vertical 
red and blue lines inside of histogram as shown in 
figures. It is observed the formation of a crystalline 
film, with small grains ranging in micrometric size 
from 0.3-1.5 m, is observed as listed in table1 while 
the grain maximum height along z-axis is lesser 
 80 nm. The orientation of grain relative to layer 
plane is nearly about 89° for the layers, 88° and 75° 
specially for cadmium and cobalt doped ones, which 
confirm the film growth along the z-axis as reported 
prior [2, 15]. The surface is lesser rough and RMS is of 
59 for undoped sample and is higher for cobalt and 
aluminium doped ones as tabulated (Table 1). 
The surface of 3%Al, 2%Sn and 3% Cd doped ZnO  
can be described as fibrous-type which might be a 
characteristic of an amorphous layer deposit as seen in 
figures 3, 4 and 7  in one hand. This trend was previ-
ously mentioned [2]. On the other hand, the 3% Sn: 
ZnO film shows a uniform texture which is formed by 
spheres as seen in 3D-view in figure 5 where the sizes 
are close, in the majority of the surface, evaluated at 
0.5 µm with a RMS roughness of 41.9 nm. 
The Figures 6 and 7 depict the Cd doped ZnO layers 
in 2 and 3D configuration and histogram distribution. 
Cobalt doped ZnO film deposited on ITO substrate 
shows two long wrinkled range of grains as seen in 
Fig. 8. The grain size and RMS variation are plotted in 
double y-axis in Fig. 9. 
 
A B C D E F G H I
0.2
0.4
0.6
0.8
1.0
1.2
1.4
1.6
 
 
  
G
ra
in
 s
iz
e
 (
µ
m
)
0
50
100
150
200
250
R
M
S
  (n
m
)
 
 
Fig. 9 – Plotting of grain size (left) and RMS (right) deduced 
from AFM analysis (A: ZnO grain A, B: ZnO grain B, C: 2 % Al, 
D: 3 % Al, E: 2 % Sn, F: 3 % Sn, G: 2 % Cd, H: 3 % Cd, I:Co)-
doped ZnO 
 
4. CONCLUSION 
 
Prepared at 1000 rpm, nanostructure of pure and 
M-doped ZnO films are synthesized and explored by the 
AFM analysis. Many details are determined by the 
microscope observation and its suitable software. 2D-
views show a non-homogenous surface with cluster and 
separated domains of grains. These latter have various 
shapes, sizes and roughnesses. Consequently, films 
more are rough 240  RMS  40 nm. The formed grain 
of layers are bigger, grain size are nano/micro metric 
(0.3-1.5 m). Based on the angle orientation of the 
grown grains around 88°-89°, we confirm the growth of 
film along the z-axis. Such as-grown layers which ex-
hibit nanostructured aspect could be utilized in micro 
and nanoelectronic devices and ferromagnetic systems 
for those doped with cobalt. 
 
 AFM CALCULATED PARAMETERS OF MORPHOLOGY INVESTIGATION… J. NANO- ELECTRON. PHYS. 7, 04012 (2015) 
 
 
04012-7 
AKNOWLEDGEMENTS 
 
The first author would like to acknowledge the head 
of virtual library SNDL https://www.sndl.cerist.dz/. This 
work was supported by ministry of high teaching and 
scientific research www.mesrs.dz and Oran University of 
Sciences and technology www.univ-usto.dz. under 
CNEPRU (2013-2016) project N°B0L002UN31022-
0130011.  
 
 
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AFM Calculated Parameters of Morphology Investigation of Spin Coated MZO (M = Al, Sn, Cd, Co) Layers

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AFM Calculated Parameters of Morphology Investigation of Spin Coated MZO (M = Al, Sn, Cd, Co) Layers

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SocioEconomic Challenges Journal (Sumy State University)