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2016 IEEE 7th Control and System Graduate Research Colloquium (ICSGRC 2016), 8 August 2016, UiTM Shah

Alam, Malaysia

High Optical Transmittance of Nanostructured TiO2


Thin Film using Dip Coating Method
S.F.A.Samat1, M.S.P. Sarah2, M.Faizul Md Idros2
Nano-Electronic centre (NET), Faculty of Electrical Engineering, University of Technology MARA, Shah Alam.
farhanizasamat@gmail.com, puterisarah@salam.uitm.edu.my, faizul_san287@yahoo.com

Abstract— Titanium dioxide (TiO2) is an universal oxide By this method the nanocrystalline structure of the material
material used in many applications such as optical sensing. improved the electro chromic device performance
TiO2 thin films have been investigated under various especially in optical sensing. The transmittance spectra,
molarities concentration by dip coating technique. The
thickness and surface roughness of the TiO2 thin films were
characterization of the thin films at different molarities of
depending on the molarities concentration of the solution.
concentrations were varied at 0.01M, 0.05M, 0.10M and
0.50M by Ultraviolet Visible Spectrometer (UV-VIS), Field This is because the surface structural increased due to the
Emission Scanning Electron Microscopy (FESEM), Atomic concentration increased. So that, the average size of
Force Microscopy (AFM) and Surface Profiler (SP). From this crystalline surface also getting bigger. Therefore, this paper
study, the optical sensing response depends on different study the optical properties of transmittance spectra,
concentrations of solution. The optical transmittance was in thickness, surface roughness, topology and morphology of
the range of 35.32% of 0.01M and 21.38% of 0.50M. The the thin films due to the molarities effect using dip coating
optical transmittance was found that increased as the technique for high optical sensing.
molarities concentration decreased. The surface structural
and the surface roughness of the thin films are also discussed.
Then the development of topology and morphology of the
Keywords— TiO2; sol-gel; dip coating method;molarities thin film characterization are measured by using FESEM,
AFM and SP for thickness. The surface roughness also was
I. INTRODUCTION recorded by AFM in the table and figures.

Titanium dioxide (TiO2) is one of the semiconductor oxide II. EXPERIMENTAL METHOD
materials that has high optical transmittance in the visible
and near-IR region, high refractive index and dielectric
constant [1] ,[2]. It has attracted wide range of applications, A. Glass substrate preparation
such as photocatalytic [3], dye-sensitized solar cells[4],
optoelectronic sensing[5] and capacitors [6]. It also has The preparation of glass substrates started with cleaning
been used abundantly in sensing application due to its process. The substrates with 2cm x 2cm dimension were
stability in photoactivity, chemically inert and biologically. immersed in beaker with chemical solution of acetone,
TiO2 were synthesized in crystalline and amorphous system methanol and deionizer water (DI) sonicated with
by sol-gel process. Sol-gel was the most efficient, ultrasonic cleaner consecutively. It took 10 minutes for
reproducibility, controllability and simple method in each step. Then, they were blown under nitrogen gas for
making TiO2 solution. drying to keep in clean substrate from other particles that
may affect their condition for next process.
There are many techniques of deposition of TiO2 thin film
such as Rf sputtering, spin coating, dip coating, chemical
B. Synthesis of pure TiO2 by sol-gel method
vapor deposition (CVD), physical vapor deposition (PVD),
pulse laser deposition and thermal deposition [7]. Dip
The preparation of TiO2 solution involved ethyl alcohol as
coating method was not expensive, efficient technique and
a solvent and titanium (IV) isopropoxide (TTIP) which acts
suitable at every substrate [8].
as precursor for synthesizing crystalline TiO2 particles.

978-1-5090-1175-9/16/$31.00 ©2016 IEEE 52


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2016 IEEE 7th Control and System Graduate Research Colloquium (ICSGRC 2016), 8 August 2016, UiTM Shah Alam, Malaysia

Glacial acetic acid (GAA) and distilled water (DI) for TTIP Figure 1 shows the optical transmittance spectra in a
hydrolysis meanwhile Triton X-100 as a surfactant. The wavelength range of 300 nm – 800 nm The transmittance is
solution was stirred and heated at 60ºC with 600rpm for the important in determining each parameter in sensing
one hour using hot plate stirrer. The solution was stirred for detection for evaluating the optical performance for
another an hour for well mixing at 30ºC. conducting oxide films. Figure 2 shows that the films are
fully transparent in the ultraviolet and it started to transmit
C. TiO2 Thin Films Deposition
in between 300 nm and 350 nm. The ultraviolet wavelength
is in the range of 8.82 nm until 390 nm. Meanwhile the
The thin films prepared by dip coating technique with visible wavelength is in range of 390 nm until 789 nm
regulation speed of 0.6cms-1. After deposited each layer, shown in Figure 2.
the substrate was undergo drying process at 100ºC in 15
minutes. The drying process was repeated until three times
and five times depends on number of layers. The drying
process is conducted to eradicate the solvent form TiO2.
Then, the thin films were annealed at 450ºC in one hour to
harden the structure.

D. The characterization of TiO2 thin films.

An Ultraviolet-Visible (UV-VIS Spectrophotometer),


(JASCO, FLH-740) is used to record the transmittance
between wavelength of 300nm and 800nm. The thicknesses
of the thin films are estimated using Surface Profiler, SP
(Dektak 150). Surface morphologies and the roughness of
the thin films are investigated using Atomic Force
Mircroscopy, AFM and the surface topology was examines
by field-emission scanning electron microscope, FESEM
by JEOL (JSM-J600F).

III. RESULT AND DISCUSSION


Figure 2: The electromagnetic spectrum of visible
A. Optical properties wavelength from 400 nm until 700 nm [9]

Figure 1: The optical transmittance of TiO2 thin films with


different molarities of (a) 0.01M (b) 0.05M (c) 0.10M and Figure 3: The optical transmittance started response at
(d) 0.50M showed the increasing transmittance as wavelength 300 nm until 800 nm with different molarities
increasing molarities. for TiO2 thin films.

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2016 IEEE 7th Control and System Graduate Research Colloquium (ICSGRC 2016), 8 August 2016, UiTM Shah Alam, Malaysia

Figure 3 shows the molarity concentration starting from It is an average size for every grain size. However, the
0.01M, 0.05M, 0.10M and 0.50M. The transmittance of grain size at 0.01M is more uniform and small than 0.05M
0.01M and 0.05M are 35.32% and 28.64% followed by shows the island surface. The Pt island covered on the Ti-O
0.10M and 0.50M are 27.39% and 21.38% respectively. particles at several peak and formed by kinetic sputtering as
Low molarities concentration gave the highest seen in the AFM images. Recent studies the Pt island was
transmittance. However the film crystalline and surface used relatively facile deposition of Pt particles onto glass
roughness increased with increasing molarities (refer Table substrates [11].
1). The surface roughness and thickness will explain in
surface topology. The thin film of TiO2 is getting saturated The grain size is in the range of 2.0 nm. The Pt island is
in increasing molarities because of the white pigments is formed from the solution that is not mixing well. Therefore
become thicker and the preferred growth of the films is the surface of 0.50M is not uniform and less porous.
changed due to a limitation of interstitial of Ti. Decreasing the molarity gave the high porosity depends on
agglomeration and denser [12]. The grain size structure of
The surface roughness and thickness are relating depends the surface at the low molarities shows the low thickness
on specula and scattered components in reflection losses and surface roughness. Meanwhile the increase thickness
that is interference phenomena reacted in chemical process and surface roughness influenced by increasing molarities.
and interference pattern [10]. Figure 3 shows the optical These will resulted the optical transmittance high in low
transmittance value at 300 nm which is the TiO2 thin film grain size and uniform.
response to visible light in short time at high transmittance
peak of 0.01M.
C. Surface Topology

B. Surface Morphology The result shows the crystalline uniformity of the TiO2 thin
films. The surface roughness was measured by AFM shows
The FESEM result in Figure 4 shows the surface in Figure 5 are the difference for each molarities are 0.01M
morphology of TiO2 thin films different on molarities (a), 0.05M (b), 0.10M (c) and 0.50M (d). The average
value. roughness, Ra for 0.01M and 0.05M are 6.303nm and
11.892 nm followed by 0.10M and 0.50M are 56.992nm
(a) (b)
and 134.421nm respectively. The roughness of the thin film
is increasing with the increasing of the molarity.

TABLE I: THE THICKNESS AND SURFACE ROUGHNESS


OF THE SAMPLE FOR TIO2 THIN FILMS AT DIFFERENT
MOLARITIES

(c) (d) Surface Morphology


Samples
Thickness(nm) Surface Roughness
0.01M 107.20 6.303
0.05M 436.87 11.892
0.10M 1264.00 56.992
0.50M 2753.70 134.421

The Figure 5 shows the topology surfaces of 0.01M is


much more uniform than the higher molarities at 0.50M,
0.10M and 0.05M.This explains the surface roughness
Figure 4: The morphological images of TiO2 thin films at increased by the increasing molarities. The surface
different molarities (a) 0.01M (b) 0.05M (c) 0.10M (d) roughness is low due to the film is quite uniform with not
0.50M with increasing surface roughness. much of porousity [13].

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2016 IEEE 7th Control and System Graduate Research Colloquium (ICSGRC 2016), 8 August 2016, UiTM Shah Alam, Malaysia

(a) (b) REFERENCES

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2016 IEEE 7th Control and System Graduate Research Colloquium (ICSGRC 2016), 8 August 2016, UiTM Shah Alam, Malaysia

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