Brazilian Journal of Physics

https://doi.org/10.1007/s13538-020-00794-3

GENERAL AND APPLIED PHYSICS

Optical-Electrical Properties and Thickness Analysis of TiO2 Thin

Films Obtained by Magnetron Sputtering
V. S. S. Sobrinho1 · J. Q. M. Neto2 · L. L. F. Lima3 · I. A. Souza2 · M. S. Libório3 · J. C. A. Queiroz2 · R. R. M. Sousa4 ·
E. O. Almeida2 · M. C. Feitor2 · T. H. C. Costa2

Received: 17 June 2020 / Accepted: 1 September 2020

© Sociedade Brasileira de Fı́sica 2020

Abstract
The study of thin films with properties that meet specific needs and improve people’s quality of life has been the focus
of many researchers. However, knowing and controlling the production techniques of these films have been a challenge
for the industry of optical-electronic devices, functional coatings, and energy conservation. The thickness of thin films is a
parameter that influences the optical and electrical characteristics of these materials, thus being one of the most important
information in the plasma deposition process. Because of the need for precision in measuring the thickness of thin transparent
films, this work proposes to evaluate the Swanepoel methods (envelope) and the PUMA, computational method, from optical
transmittance curves and compare them with the measurements directly made by microscopy. Scanning electronics for thin
films of TiO2 deposited by magnetron sputtering in different conditions. The results of this study showed that the PUMA
method is capable of calculating film thicknesses of a few hundred nanometers and with few interference fringes. The PUMA
method showed convergence with high precision for films produced with 30 and 60 min of treatment and a difference of
17% for films with 120 min of deposition concerning the measurements made by microscopy.

Keywords Thin films · Magnetron sputtering · Swanepoel method · PUMA · Transmittance

1 Introduction Several techniques can be used to obtain the thickness

Industrial advances have increased interest in the develop-
ment of thin films and new technologies based on nano-
materials that have resulted in a series of applications to
improving people’s lives. Thus, the application of thin films
extends to optical-electronic devices, functional coatings,
and energy generation and conservation [1]. Works have
been produced analyzing optically thin films of the most
diverse materials and demonstrating the influence of the
thickness of such films on their optical properties [1–5].
The optical analysis of thin films is for determining the
optical and photocatalytic properties of the materials [6–
9], with the material thickness being deposited information
necessary to obtain the absorption coefficient of the films
and their Bandgap. Therefore, the use of accurate methods
to obtain this measure is essential for the study of these
materials.
 M. S. Libório
maxwellsantana@ect.ufrn.br
Extended author information available on the last page of the article.
of thin films: such as profilometry, ellipsometry, cross-
sectional SEM, and optical analysis [10, 11]. As optical
analysis has the advantage of being a non-destructive
method and depends only on the output data of a
spectrophotometer to obtain thickness values. In this
perspective, the method most used in the literature for
this analysis is still the Envelope Method, created by
Manifacier and collaborators [12–16]. The success in using
the Envelope method in the optical analysis of transparent
thin films and the calculation of the thickness value is
related to the low error of the measurements for micrometric
films and the fact that only the percentage values of the
transmittance of the film are used as input data, obtained by
a spectrophotometer [12, 16, 17].
The optical analysis method proposed by Swanepoel
(1983) [18] is a precise method for calculating all thin
film optical constants, which is an advantage since not all
spectrophotometers provide the reflectance values of films.
However, it is essential to highlight the limitations of this
method. First, the films must be thin, that is, their thickness
must be many orders of magnitude less than the thickness
of the substrate that holds it [19]. The substrate must be

transparent in the region of analysis, that is, resulting in a
region of weak and medium absorption in the transmittance
graph [19]. For the application of the Swanepoel method,
the transmittance graph must present interference fringes.
This phenomenon occurs when the film is uniform and not
very thin (a few tens of nanometers) [20]. On the other hand,
when they are deformed, in general, they do not have fringes
due to the variation in their thickness, causing destructive
interference in the light output of the film. For this reason,
research [16, 17, 21–25] to propose improvements in the
method proposed by Swanepoel for increasingly accurate
measurement of the thickness and optical properties of thin
films are increasingly common, regardless of how these
films were produced.
As with the Swanepoel method, the PUMA Compu-
tational Method (Pointwise Unconstrained Minimization
Approach) [26] is also a way of determining the optical
parameters of the film by finding a theoretical transmit-
tance function dependent on the incident beam wavelength
(λ), the refractive index of the substrate (s), refractive film
index (n), film thickness (d), and film absorption coefficient
(α) [18]. Your problem is to obtain T theor = T exp , for each
wavelength value. This solution must contain the smallest
standard deviation between the theoretical and measured
values so that the results are optimized. This method proves
to be extremely useful and reliable for estimating film thick-
ness when using four-digit transmission data [27]. The great
challenge of this computational method is to provide pre-
cise values of thickness in analyzes of optical transmittance
spectra, mainly when the samples are considerably thin
films and with a high value of optical absorption coefficient
[28]. Theoretical methods, based on different mathemati-
cal devices, are recurrent in the literature [7, 13, 19, 28–32]
seek to obtain the lowest percentage of error concerning the
determination of thickness.
Manthrammel et al. [33] proposed a method based on
Kramers-Kronig relations to estimate the values of the
index of refraction and extinction of thin films based on
pink dye RsB. The authors found that the results are
improved by increasing the thickness of the films, but
they did not show the same performance with very thin
films. The computational method provides good recovery of
transmission data where other methods fail, such as in very
thin films or more absorbent layers.
Table 1 Deposition parameters for TiO2 thin films
Samples O2 (cm3 /min)
A1 3.0
A2 2.5
A3 2.5
A4 2.5
Braz J Phys
Liu et al. [34] calculated using experimental method
way the optical constants of thin films of CdS deposited
by a chemical bath at different temperatures. It has been
suggested that the increase in temperature promotes phase
transformations and variation in the crystallinity of the
films. The authors concluded that there is an inverse
relationship between film thickness and packing density
with transmittance. These results were later corroborated
by Khatibani, Bagheri, and Rozati [35], who, using
PUMA, theoretically calculated the optical constants of thin
prepared by spray pyrolysis. The same inverse relationship
between thickness and packing density of the films was
observed with the transmittance and confirmed with the aid
of SEM images.
In this work, a comparative analysis will be carried out
between the thickness results obtained for thin films, of a
few hundred nanometers, by the Envelope Method and by
the PUMA, Computational Method, applied to the study of
TiO2 films deposited in plasma by magnetron sputtering.
This methodology proposes to find the thickness and optical
constants of TiO2 thin films by approximation and to
generate a theoretical curve for the transmittance function
comparable with the real transmittance curve obtained by
the spectrophotometer. Therefore, the approximation of the
curves characterizes the feasibility of applying the method
under the conditions studied.
2 Materials and Methods
Glass slides of 1-mm thickness were used for the deposition
of TiO2 films. The slides were cleaned by ultrasonic
agitation, being used for cleaning, distilled water, isopropyl
alcohol, and acetone, respectively. The films were deposited
by Magnetron Sputtering, using a target in the form of pure
titanium tablets, with a diameter of 61 mm and a thickness
of 1 mm. All depositions were made with 5.0 cm3 /min of
Air, 0.45 A (current), 100 Hz (frequency), and a distance of
60 mm between the titanium target and the sample holder.
However, the study focused on the changes caused by the
variation in the O2 flow and time of treatment. Variable
deposition parameters are shown in Table 1. Each parameter
was repeated in three glass samples so that a total of twelve
samples were studied.
Time (min)
30
30
60
120
Braz J Phys

Fig. 1 Appearance and coloring of thin TiO2 films under visible light

The parameter of 3.0 cm3 /min of O2 flow was not of TiO2 thin films were estimated through the relationship
used for time of 60 and 120 min because no significant between the absorption coefficient (α) and the photon
changes were observed in the results. The transmittance energy (hν) [18]. Doing a linear regression in the region
analysis of the films was performed using a Genesys 10- with a constant slope of the curve [α(hν)]2 × hν and
uv spectrophotometer, from the Thermo Fisher Scientific extrapolating this regression to the energy axis (in which
brand, with a scan from 190 to 1100 nm and a step of 1 in the value of α is zero), we have the optical gap value for
1 nm. For XRD analysis, a Bruker D2 Phase diffractometer each film.
with copper Kα radiation (λ = 1.54 Å), 2θ intervals between
20◦ and 70◦ , 0.01◦ step, 10 mA current, was used at a
voltage 30 kV, using a Lynxeye detector. For cross-sectional 3 Results and Discussion
examinations of the film, SEM was used using a Hitachi
Tabletop Microscope TM300 bench microscope. Figure 1 shows the change in the visual aspect of thin TiO2
With the transmittance data acquired by the spectropho- films due to the variation in the oxygen flow and deposition
tometer, the Envelope method (Swanepoel, 1983) and the time. Regarding the influence of the angle of incidence of
PUMA Computational Method were used to obtain the light on the composition of colors present in the thin film,
thicknesses of the TiO2 films. The transmittance is a func- this is invariant, according to Park et al. [39].
tion of the λ wavelength, the thickness d, the refractive
index n, and the α absorption coefficient of the film,
the last two optical properties being unknown functions
of the wavelength. Therefore, the PUMA software esti-
mates the thickness d, the refractive index n (λ), and
the alpha absorption coefficient α(λ) from the resolu-
tion of the nonlinear system of equations, as shown in
(1) [36, 37]:

T exp (λi ) = T theor [λi , d, n(λi ), α(λi )] f or i = 1, ..., m

(1)
After applying the methods, the absorption coefficient
of the films was determined by the Beer-Lambert Method
[38]. For the 120 min films, the Envelope Method was
also used for the purpose of comparing the behavior of
the curves for the functions of the coefficient found, and
then the Bandgap of the films by the Tauc method was Fig. 2 Diffractograms of TiO2 thin films deposited on glass with
found. Through optical spectroscopy, the Bandgap values different treatment conditions

Fig. 3 Transmittance curves of
the groups of 3 samples with
TiO2 films for the different
treatment conditions
It is observed that the samples with a longer deposition
time turned yellow. Thin TiO2 films have a yellowish color
when most of their structure is composed of a rutile phase
(dark yellow), which is a phase with better light spreading
efficiency, or anatase phase (light yellow), which is an
associated phase the best photoactivation [28].
The blue color of the A1 and A2 films explains the
lack of time for the nucleation of the particles deposited in
the growth stage of the film, resulting in the formation of
Fig. 4 A4 sample transmittance (120 min) using the envelope method
Braz J Phys
smaller nuclei. This observation is in line with the results
obtained by Hanaor and Sorrell [27]. Films with different
thicknesses show color changes. However, the magnetron
sputtering deposition technique is used for the production
of uniform thin films (with low thickness variation) [40].
Therefore, it is concluded that the color variation in the same
film is the result of the presence of different TiO2 phases.
Fig. 5 Refractive index of pure glass and thin film of TiO2 deposited
with 120 min
Braz J Phys
Fig. 6 Comparison between real transmittance curves and recovered
by PUMA for a 120-min and b 30-min film depositions
In Fig. 2, the XRD spectrum is observed for samples with
TiO2 deposition. Although the analysis is performed with
an angle of incidence of 3◦ , the amorphous phase from the
glass substrate is evident in the lower scanning angles. This
behavior is in line with that observed in the literature [6,
15, 22]. When analyzing thin films deposited on atomically
disordered material with XRD, it is common to obtain
information on the amorphous character of the substrate,
making it difficult to sharpen the peaks presented. For the
120-min treatment, the presence of TiO2 is observed due to
the rutile peaks in the orientations (110), (101), and (210)
and anatase in the orientation (101), which is a characteristic
orientation for anatase nanocrystals [34]. Traces of rutile
(110) are observed in all deposited films, having also found
TiO2 (100) and (002) in the 60-min film, TiO0.5 (001) in the
30-min film A1, and the semiconductor oxide Ti3 O5 (202)
in the films of 120 min and 30 min A1 [11, 21].
From the DRX results presented, it is observed that, with
the increase in the deposition time, there was a tendency to
form films with more crystalline structure, rutile and anatase
compounds in the orientation (110), which was expected
due to the presence of the presence of yellowish color for
these films.
The transmittance spectra with the interference curves
are represented in Fig. 3. The films deposited after 120 min
showed a higher number of interference fringes. Therefore,
the Swanepoel Method for determining its thickness was
applied only to these films, since this method requires
a higher number of fringes to produce reliable results
[19]. This standard is suitable for TiO2 film applications
as semiconductors due to low Bandgap values. All other
films have few interference fringes, probably due to the
the small thickness of these films. Therefore, for the
Table 2 Mean squared error (MSE) between the theoretical curve obtained by PUMA method and the real transmittance curve
Samples
A1
A2
A3
A4
analysis of the 30-min (A1 and A2) and 60-min films, the
PUMA, Computational Method, was used, in addition to the
120-min deposition films.
The Envelope Method was used to find the optical
constants and then the film thickness of 120 min. Figure 4
shows the transmittance graph, already enveloped, for one
of the 120-min samples. A T M function that contains the
maximum interference points and a T m function with all
the minimum interference points are found with polynomial
extrapolation of the maximum and minimum points of
the interference fringes, generating a packaging of the
Transmittance (T) function.
To apply Swanepoel’s method, the refractive index of the
glass substrate and the film were found, as shown in Fig. 5.
The results show an increase in the refractive index of glass
with film (120 min) from 1.51 to approximately 2.15.
Figure 6 shows the approximation between the trans-
mittance curve obtained by the PUMA method and the
curve obtained by the spectrophotometer for samples A1
and A4, with 30 and 120 min of treatment, respectively.
These graphs show that the computational method gener-
ated a curve, in the range of 500 to 850 nm of wavelength,
with a high approximation to that obtained by optical spec-
trophotometry. The use of the PUMA computational method
allows obtaining a transmittance curve close to the real one
from estimates of thickness and values of optical parame-
ters.
The mean quadratic error (MSE) between the curves
is the reliability criterion of the computational method.
The results showed low error values for films A1, A2,
and A3, which proves the efficiency of the method as a
solution for calculating the thickness of thin films that
have few interference fringes (an unviable condition for the
application of the Envelope method). For sample A4, with
a thin film of TiO2 deposited in 120 min, an approximation
with quality slightly lower than those found in other samples
was obtained, however, sufficient to represent the real
transmittance curve with reliability. The film of sample
A4 has more interference fringes, with more considerable
variation in the points measured by the spectrophotometer.
Therefore, this variation results in greater difficulty for the
PUMA method algorithm to find a theoretical transmittance
function close to the real curve. The MSE values for each
TiO2 thin films are shown in Table 2.
MSE × 10−5
1.20
2.04
1.15
3.28

Fig. 7 Transverse SEM of glass
samples with TiO2 film. a A1. b
A2. c A3. d A4
Figure 7 shows the cross-sectional images of the
thin films and TiO2 obtained with a scanning electron
microscope to measure the thickness of the deposited
layers. The micrographs show homogeneous and continuous
depositions of the films due to the high flatness and low
roughness of the glass substrate surface.
Table 3 shows the comparison between the results of
thickness measurements performed by SEM, calculations
obtained by the Envelope method (Swanepoel), and using
the computational method PUMA with their respective
standard deviations of the measurements. Due to the small
number of fringes presented by samples A1, A2, and A3,
it was not possible to obtain the thickness values for these
films. The results presented by the PUMA method for the
measurement of the thin film thickness of TiO2 agree with
the values measured by the scanning electron microscopy
technique for films obtained with 30 and 60 min. For the
film obtained after 120 min, there is an average difference
of 17% between the measurement obtained by SEM and the
PUMA method. However, the difference in relation to the
Table 3 Comparison between all thickness measurements found for TiO2 films
Samples SEM
A1 114±8
A2 113±14
A3 209±15
A4 369±12
Braz J Phys
40% envelope method shows that the computational method
produces better convergence between the studied methods.
The film, with the most different thickness measurement,
analyzed by the PUMA method, was that of 60 min
of deposition. However, when standard deviations are
taken into account, the error can be reduced considerably.
The thickness values for the 30-min films (A1 and A2)
did not show variation in their thickness in relation to
the measurements made by SEM, which means that the
variation of 0.5 cm3 /min in the oxygen flow did not cause
the modification of coating thickness.
Figure 8 shows the Bandgap results obtained by the
Tauc method for all films produced in this work. For the
application of the method, it was necessary to calculate
the absorption coefficient for the TiO2 films deposited
from the transmittance graphs. For the 30-min films (A1
and A2), there were no significant variations in their
Bandgap, which shows that the variation in oxygen flow
from 3.0 to 2.5 cm3 /min does not cause significant
changes in the photocatalytic property of the coating. As
Swanepoel PUMA
Thickness (nm)
− 107±5
− 102±10
− 142±42
512±30 432±23
Braz J Phys

Fig. 8 Bandgap of TiO2 thin

film. a A1. b A2. c A3. d A4

previously mentioned, there was no significant variation in
the thickness of film tests, which justified, in this work, the
option of depositing all other films with only 2.5 cm3 /min.
It is noted that all values for Bandgap (Table 4) are in
line with what was expected according to the literature since
the XRD results (Fig. 2) showed more crystalline films
deposited to 120 min It is known that for pure TiO2 films,
the higher the crystallinity of the coatings, the lower the
Bandgap values, with crystalline films expected to be close
to 3.10 eV [41].
However, the Bandgap values showed dependence on the
crystallinity and thickness of the coatings, concluding that
the control of these factors is fundamental for the creation
of films with photocatalytic properties.
4 Conclusions
The deposition parameters used in this study resulted in
thin transparent TiO2 films with high optical transmittance.
Among the films analyzed, those deposited in 120 min
showed a more crystalline structure, this statement being
confirmed by the phases verified by the DRX and by the
Bandgap values of these films. On the other hand, the
samples produced with a time of 30 and 60 min showed a
more amorphous structure. Among the methods of optical
analysis, the Computational Method obtained thickness
results closer to those obtained by SEM, even for the
films of 120 min of deposition, which can be justified
by the small number of fringes that all deposited films
presented, a crucial factor for the success of the Envelope
Method.
The PUMA, Computational Method, can be used to find
the thickness and optical properties of thin films even when
they have few interference fringes.
The Bandgap of the thin TiO2 films analyzed showed
dependence on thickness and crystallinity. The understand-
ing and control of these factors in the plasma deposition
process can be used for the development of films for spe-
cific applications with transparent and conductive films

Table 4 Bandgap values found for all samples

Samples Bandgap (eV) Average (eV) Standard deviation (eV)

G1 G2 G3

A1 3.34 3.35 3.35 3.35 5.8 × 10−3

A2 3.33 3.37 3.37 3.36 2.3 × 10−2
A3 3.32 3.30 3.30 3.31 1.2 × 10−2
A4 3.13 3.18 3.10 3.14 4.0 × 10−2

with desirable photocatalytic or photo and electro activation
characteristics.
Compliance with Ethical Standards
Conflict of Interest The authors declare that they have no conflict of
interest.
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Affiliations
V. S. S. Sobrinho1 · J. Q. M. Neto2 · L. L. F. Lima3 · I. A. Souza2 · M. S. Libório3 · J. C. A. Queiroz2 · R. R. M. Sousa4 ·
E. O. Almeida2 · M. C. Feitor2 · T. H. C. Costa2

V. S. S. Sobrinho
valmar.sobrinho@ifrn.edu.br
J. Q. M. Neto
quinzinhomedeiros@gmail.com
L. L. F. Lima
tutulima@ufrn.edu.br
I. A. Souza
ivanalves@ufrn.edu.br
J. C. A. Queiroz
avcesar6@gmail.com
R. R. M. Sousa
romulorms@gmail.com
E. O. Almeida
fis777@ufrn.edu.br
M. C. Feitor
mcfeitor@gmail.com
T. H. C. Costa
thercioc@gmail.com
1 Physics Department, Federal Institute of Technological Education,
Natal, Brazil
2 Department of Mechanical Engineering, Federal University of Rio
Grande do Norte, Natal, Brazil
3 School of Science and Technology, Federal University of Rio
Grande do Norte, Natal, Brazil
4 Department of Mechanical Engineering, Federal University of
Piauı́, Teresina, Brazil