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Optimization of Electrical and Optical Properties of Indium Tin Oxide Thin Films Prepared by
Magnetron Sputtering
Muslimin1* , M. Ainul Muslim1, M. Fi Ailal Muslim2
1,2,3.
Dept. of Physics education, Tadulako University, Central Sulawesi, 94119, Indonesia
2
Graduate students of science at Tadulako University, Central Sulawesi, 94119, Indonesia.
3
Students of the Faculty of Medicine at Tadulako University, Central Sulawesi, 94119, Indonesia

Corresponding Author Email: fisikamuslim@[Link]

ABSTRACT

Indium tin oxide (ITO) is considered one of the most interesting physical properties to be
Keywords: studied. The properties of the ITO material are heavily influenced by deposition
Oxygen partial pressure Annealing Structure techniques and post-deposition treatments. The deposition of the ITO thin film was
Elektrical and Optical properties carried out using DC sputtering by varying the partial oxygen pressure during deposition
and applying different annealing temperatures to the samples. X-ray analysis revealed
that all the samples exhibited a maximal orientation of the (400) plane. Structural analysis
results showed that the lattice constant ranged from 10.17 to 10.25 Å, while the grain size
ranged from 109.10 to 122.81 nm. Both the lattice constant and grain size decreased as
the partial oxygen pressure and annealing temperature increased. Electrical resistivity,
carrier density, mobility, and bandgap were also found to change with higher partial
oxygen pressure and annealing temperatures. The carrier density ranged from (2.77–6.89)
x 10²⁰ cm⁻³, mobility from 19.63–32.98 cm²V⁻¹s⁻¹, bandgap from 3.78–4.30 eV, and
resistivity from (3.67–9.7) x 10⁻⁴ Ω•cm, with the lowest resistivity achieved at 3.70%
oxygen partial pressure and an annealing temperature of 250 °C. Optical properties also
showed changes, including the refractive index (2.09–2.25), damping constant (2.93–
3.49), absorption coefficient (0.036–0.072), and transmittance (81.94%–87.12%). The
highest transmittance was observed at an oxygen partial pressure of 8.90% with an
annealing temperature of 250 °C.
1. INTRODUCTION simultaneously introduced through a flow meter until the
pressure reached 2 x 10⁻³ mBarr. The partial pressure of oxygen
The electrical properties of the thin film In₂O₃: SnO₂ introduced during each deposition was the ratio of argon gas
(indium tin oxide), more commonly known as ITO, are pressure to oxygen gas pressure, with values of 2.50%, 3.70%,
strongly influenced by the deposition parameters and the 5.10%, 6.15%, and 8.9%, respectively, for each sample.
degree of crystallinity of the formed layer [1]. The Sn doping Annealing was conducted in a vacuum chamber at a pressure of
in the formed crystals is affected by the degree of oxygen 10⁻³ mBarr for 60 minutes at temperatures of 175 °C and 250 °C
deprivation during deposition [2]. As a donor, Sn is for each sample.
substituted for In atoms, serving as a source of extrinsic The thin film thickness was calculated based on the reflectance
charge. Two key factors contributing to the free charge in the measurements from the UV-Vis results at a wavelength range of
ITO thin layer are oxygen vacancies and the substitution of 350–800 nm [15]. Microstructure analysis was conducted using a
Sn atoms for In atoms. Oxygen vacancies result in the Philips Analytical Diffractometer PW 3710 X-ray diffractometer
production of two free electrons, while the substitution of Sn with a Co anode tube. The diffraction angle (2θ) ranged from 20°
atoms for In atoms generates one free electron [3]. to 70°, and the peak positions in degrees, along with the Full
A thin film of oxygen-depleted ITO is formed as a group Width at Half Maximum (FWHM), were identified as key
consisting of free atoms of In and Sn, along with black oxides indicators [16]. The crystal size, lattice distortion, grain size, and
InO and SnO. The formation of black oxide groups in the lattice constants were determined from the XRD results [17].
ITO thin film may result in reduced transparency of the layer The electrical properties were analyzed using four-point probes,
[4]. The amorphous ITO layer is quickly crystallized at a as shown in Fig. 2. Carrier concentration, charge carrier mobility,
temperature of 150 °C, with changes to its electronic and band gap were determined using various equations. The
structure occurring at a temperature of 135 °C [5]. The grain optical properties of the ITO were measured using UV-Vis, with
size is increased as the annealing temperature rises. reflectance, transmittance, attenuation constant, and absorption
The electrical and optical properties of ITO are strongly being calculated from the UV-Vis results using specific equations.
influenced by a high degree of crystallinity [6]. Oxygen
deficiency prior to deposition occurs because, during the
deposition process, the oxygen in the In₂O₃ and SnO₂
compounds is released first, as the boiling point of oxygen is
lower than that of In and Sn, leading to oxygen depletion [7].
The lack of oxygen during deposition can prevent the
complete oxidation of In and Sn atoms [8]. These
occurrences affect the structure, electrical properties, and
optical properties of the resulting thin films [9]. The addition
of oxygen from an external source during deposition allows it
to bond with In and Sn atoms, forming oxide compounds
[10].
flow, resulting in an electric current.
In and Sn atoms that are electrically inactive in their
inserted positions can be activated through annealing [11].
The electrical and optical properties of the ITO thin Figure 1. dc sputtering instrument.
film are influenced by the amount of Sn doping relative
to In and the rate of oxygen deprivation in In₂O₃ [12].
The structure, electrical, and optical properties of ITO
can be optimized by modifying the deposition
parameters, such as the oxygen partial pressure, and by
annealing to adjust the density of the charge carriers and
their mobility. Therefore, the addition of oxygen during
deposition and annealing is regarded as an effective
method to enhance the charge carrier density and
mobility in ITO thin films [13]. The degree of
transparency of the ITO layer is determined by the partial
oxygen pressure. The energy band shift observed in the Figure 2. Four-point probes instrument.
absorption curve can be attributed to variations in the
number of oxygen vacancies in the formed thin films
[14].
2. EXPERIMENTS

The ITO thin films were fabricated using DC sputtering

PK 75 with a rotary Trivac D 665 B and a 1000/1500
Turbotronic rotary pump, as shown in Fig. 1. The samples
were analyzed using XRD and UV-Vis-NIR measurements,
Hall Effect analysis, and four-point probe testing.
Deposition was performed with optimizations in the
percentage of partial oxygen pressure and annealing after Figure 3. Hall effect measurement.
deposition. The deposition was carried out in a vacuum The measurement of the ITO crystal microstructure was
chamber with a pressure of 10⁻⁵ mBarr. The sputtering characterized by X-ray diffraction, primarily for grain size, lattice
process was initiated while argon gas and oxygen gas were constants, and crystal orientation. The obtained crystals exhibited
the orientation of the hkl plane (400), as shown in Fig. 4. 0,9 𝜆
The grain size (G) and lattice constants were calculated at 𝐺= (1)
𝛽 cos Ɵ
the maximum orientation angle of 2θ, approximately 40.9°. Where λ is the X-ray wavelength, β is the FWHM in radians,
and θ is Bragg’s angle.
The change in grain size is attributed to the oxygen vacancy
rate and the diffusion rate resulting from the annealing
temperature. The entire layer is perfectly crystallized into fine
grains with a size range of (68.99–122.76) nm. This average size
increases to 112.09 nm for annealing temperatures of 175 °C and
117.06 nm for annealing at 250 °C. The change in crystal grain
size at temperatures between 175 and 250 °C due to annealing
has not changed significantly, as most of the free atoms have
undergone diffusion.
The results obtained show that indium amorphous oxide will
generally crystallize rapidly at a temperature of 150 °C. As
crystallization progresses, the entire layer becomes filled with
granules that are almost perpendicular to the surface [24].
Annealing temperatures allow the crystals to grow larger and
reach the surface, eventually touching each other on the surface
and leaving behind the amorphous region [25].
The grain size is almost the same as that obtained by [26], with
Figure 4. X-ray diffraction patterns of ITO film for values ranging from (100–460) nm at temperatures of (423–473)
different K and sizes of (35–50) nm at 350 °C with 5% by weight of Sn.
partialoxygen pressure. The lattice constants obtained were 11.9 nm at a substrate
The resulting XRD pattern of the ITO coatings is temperature of 600 °C [27].
crystalline, with a tendency to exhibit a (400) orientation The conversion of lattice constants can be analyzed using the
[18]. The orientation of the diffraction coating plates is Cohen method [28].
consistent across all variations in oxygen content, indicating ∆𝑑 ∆𝑎
significant compatibility with the bulk cubic structure data of = = 𝛫 𝑐𝑜𝑠 𝜃 (2)
𝑑 𝑎
In₂O₃. The highest intensity occurs at the angle (2θ) of 40.9°, 𝑎
𝑑ℎ𝑘𝑙 = (3)
corresponding to the (400) reflection of the body-centered √ℎ2 + 𝑘 2 + 𝑙 2
cubic (bcc) structure. The intensities of the (400) and (222) Where the lattice size is denoted as "a," the lattice constant is
reflections stand out against the background intensity, "Κ," which is a constant of 0.9, and "hkl" represents the preferred
suggesting that the material structure has already orientation.
crystallized, as indicated by the smaller FWHM. It is The smallest lattice constant of 10.17 Å was observed at an
believed that the shape of this diffraction pattern results from oxygen partial pressure of 6.15% and annealing at 175 °C. The
the deposition temperature, which causes the material to results of the lattice analysis show lattice distortion, including
transition from the amorphous region [19]. both shrinkage and widening, due to the influence of oxygen
The XRD pattern indicates that maximum intensity occurs partial pressure and annealing temperature. The lattice constants
in the (400) plane, with a tendency for increasing oxygen of the above samples are quite good when compared to the ITO
levels. The increasing intensity of the diffraction pattern and value from the ASTM card of 10.118 Å. The shrinkage in the
the reduction of FWHM are attributed to the rise in oxygen grating parameters obtained is considered quite good because it is
vacancy concentration and the diffusion rate resulting from relatively small, ranging from approximately (0.052-0.212) Å.
annealing in the deposited layer. This change is due to the The crystal lattice constant shows a downward trend when the
reduction of In-free atoms and Sn impurities as they are oxygen partial pressure increases [29]. This change is associated
oxidized by the oxygen introduced during deposition. with the distortion occurring in the crystal due to point defects
Oxygen from In₂O₃ and SnO₂ compounds is initially caused by oxygen atoms, which are relatively small compared to
deposited because the boiling point of oxygen is lower than the radii of In and Sn, approximately 1.509 Å [30]. This local
that of In and Sn, leading to oxygen deficiency. distortion acts as an additional scattering center for the electron
The intensity of the diffraction pattern shows an current flowing through the crystal, resulting in increased
increasing tendency, and the full width at half maximum resistance.
(FWHM) decreases in samples annealed at 250 °C, which The lattice construction is changed due to strains, which are
enhances the intensity and narrows the maximum half-peak influenced by the contribution of oxygen vacancies. The effects
width [20]. A peak with maximum intensity is obtained in of oxygen partial pressure during deposition are significant, with
the (222) field, with the orientation of the plating (400) at consistent changes observed in the lattice, while the lattice
26° and the plane (400) at the deposition temperature of 350 constant is decreased as the annealing temperature rises due to
°C using the electron beam method. Additionally, it is the Sn/In ratios becoming smaller [31]. The decrease in lattice
explained that amorphous indium oxide generally constants is attributed to the microstrain effect and elastic strain
crystallizes rapidly at a temperature of 150 °C with HDPE in caused by impurities and vacancies [32]. The results of the
the (222) field. analysis of the ITO thin film structures are shown in Table 1.
In general, the widening of the peak in the X-ray
diffraction pattern of a crystal sample is influenced by the
size of the crystal and the microstrain effect [21]. The
diffraction peak width is assumed to result from the small
crystal size rather than from lattice strain [22].
The crystallite size was calculated from the XRD pattern
using the Debye-Scherrer formula [23].
 Table 1. The structural parameters of the prepared ITO thin films for different partial oxygen pressures and annealing conditions.

Oxygen Lattice
Annealing 20 Intensity FWHM Grain (hkl)
Partial hkl Constant
(°C) (deg) (Max) (deg) (nm)
(%) (Å)
175 41.065 400 0.16 400 10.25 122.81
2.50
250 40.955 729 0.16 400 10.23 122.76
175 40.880 745 0.18 400 10.24 109.44
3.70
250 41.250 686 0.16 400 10.21 122.80
175 41.060 729 0.18 400 10.21 109.51
5.10
250 40.910 226 0.18 400 10.21 109.10
175 41.180 325 0.18 400 10.17 109.55
6.15
250 35.345 350 0.16 222 10.19 120.70
175 41.060 747 0.18 400 10.20 109.16
8.90
250 41.135 1102 0.18 400 10.21 109.95
into the intrinsic band if the concentration of impurities continues
3.2. ELECTRICAL STUDIES to increase.
Another effect that arises as a consequence of the increase in
Indium Tin Oxide is a compound doped with Sn. The Sn impurity concentration is the formation of impurity energy bands
atom doping can function as a substitute for one of the atoms that can affect the energy bands. This impedance causes the
in the main In₂O₃ crystal, or it can position itself at an lower energy band to expand, resulting in a narrowing of the
insertion site. Sn atoms can also form bonds with oxygen, energy bands (tail band effect).
such as SnO or SnO₂, depending on their valence state of +2 The price estimates of critical density donors can be
1
or +4. The Sn⁴⁺ state in SnO₂ can function as an n-type 3 ∗ ∗ ℎ2𝜀0 𝜀 𝑀
donor, with electrons being released into the conduction determined by the Moott criteria, 𝑛 𝑐 𝑎0 ≈ 0,25where 𝑎0 = 𝜋𝑒 2 𝑚∗𝑐
energy band. , 𝜀 is the static dielectric constant of the parent lattice (𝜀 𝑀 =
𝑀

As the concentration of Sn doping atoms increases, the 𝜀 𝑙𝑛2 𝑂3 (𝜔

̅ = 0) = 8,9). The effective mass in the conduction
electron wave functions at the impurity level will overlap band is (𝑚𝑐∗ = 0,35𝑚𝑒 ) with a Bohr radius 𝑎0∗ ≈ 1,33 𝑛𝑚.
with each other. The occurrence of this overlapping effect
causes changes in the potential of the energy levels of each
electron, resulting in the formation of a band of energy levels
in the area. The impurity energy band will widen and merge
Table 2. Electrical parameters of ITO thin films for different oxygen partial pressures and annealing conditions.
Oxygen
Annaeling Resistivity Density (n) Mobility (μ) Energy
Partial
(oC) (× 10 𝑐𝑚 )
−4 −3
(× 10 𝑐𝑚 )
20 −3
(𝑐𝑚 𝑉 𝑠
2 −1 −1
) Gap (eV)
(%)
175 5.50 5.39 21.49 3.92
2.50
250 3.67 6.03 28.24 3.81
175 4.89 6.51 19.63 4.29
3.70
250 3.06 6.89 29.64 3.92
175 7.34 3.38 25.19 4.20
5.10
250 4.89 3.88 32.94 3.78
175 9.17 3.05 22.35 4.30
6.15
250 6.11 3.25 31.47 4.10
175 9.78 2.77 22.86 4.35
8.90
250 6.72 2.82 32.98 4.20
The structure of the energy band of indium tin oxide with electrical conductivity σ can be expressed by the equation.
high doping density is shown, 1
𝜎 = 𝑒(𝜇𝑛 + 𝜇ℎ 𝑝) (6)
𝐸𝑐 (𝑘) = 𝐸𝑐0 + ħ Ʃ𝑐 (𝑘) (4) 𝜌
𝐸𝑣 (𝑘) = 𝐸𝑣0 + ħ Ʃ𝑣 (𝑘) σ is the electrical conductivity, and ρ is the electrical resistivity.
𝐸𝑣 (𝑘) is the valence energy with doping, and 𝐸𝑐 (𝑘) is the The resistivity of thin films to oxygen partial pressure and
conduction energy with doping. annealing is shown in Fig. 5. The lowest resistivity of the ITO
The density and mobility of electron carriers in extrinsic thin film was obtained at a partial oxygen pressure of 3.7% with
semiconductor loads are influenced by the availability of free annealing treatment at a temperature of 250°C. This resistivity is
electrons. related to the load carrier density, which is 6.89 x 10²⁰ cm⁻³, with
4𝑒 𝜋 1⁄3 −2 a charge carrier mobility of 29.64 cm²/V·s and a band gap of 3.92
𝜇 = ( ) ( ) 𝑛 ⁄3 (5) eV.
ℎ 3
μ is the carrier mobility, and n is the electron density. The ITO thin films made at the same oxygen partial pressure but
with different annealing treatments will result in different boundaries.
resistivities. Meanwhile, the resistivity of the ITO thin film The change in electrical resistivity of the ITO layer after
made at a 3.7% oxygen partial pressure with annealing at a annealing is caused by the diffusion process of oxygen and the
temperature of 175°C was higher than that of the thin film opposite diffusion of Sn. Oxygen diffusion leads to the diffusion
annealed at 250°C.
of oxygen atoms into the ITO thin films, resulting in a decrease
in the density of oxygen vacancies during the annealing process.
On the other hand, Sn diffusion involves the movement of Sn
atoms from the grain boundaries and insertion sites to the lattice
sites of In₂O₃, forming SnO₂ oxide. Generally, donors from Sn
are activated after reaching a certain temperature, causing the
free electron density of the ITO thin layer to increase
significantly, as shown in Fig. 6.

Figure 5. Resistivity as a function of oxygen partial

pressure and annealing.

a This is related to the level of crystallinity. This can be

seen with the smaller carrier density obtained, which is 4.86 x
10²⁰ cm⁻³, and a mobility of 34.02 cm²/V·s.
The change in density and charge carrier mobility is the
result of the contribution of free electrons to indium tin
oxide, derived from the diffusion of impurity atoms Sn+4 Figure 6. Shows the resistivity, density, and
replacing Sn+3 atoms in the In2O3 parent lattice, according to mobility at an annealing temperature of 250 °C.
equation (4). The electron contribution originating from Sn, The decrease in density at an oxygen partial pressure of 3.7%
due to its bonding with oxygen and replacing the In atom in is due to the formation of InO, SnO, and free In and Sn atoms,
the In2O3 lattice, is related to the carrier density, which which function as impurities that act as scattering centers for
causes a change in electrical resistivity. The mentioned ions.
changes are also due to the free electrons from In and Sn Electrical resistivity decreased to 3.06 x 10-4 Ω cm at an
atoms that are unable to oxidize because of the increased oxygen partial pressure of 3.70% then increased to 6.72 x 10-4 Ω
concentration of oxygen vacancies during deposition. During cm at oxygen partial pressure of 3,70%-8,90%, with an annealing
deposition, the In2O3 compound releases some oxygen, temperature of 250 oC. The change in the density and mobility of
resulting in a different composition, initially In2O3-x (Vo")xe2x the charge carriers due to the oxygen vacancies in In is mitigated
, where Vo" represents the oxygen vacancy with two when the addition of oxygen from the outside reaches 3.70%.
electrons, and e2x' represents the electron needed to 3.3. OPTICAL STUDIES
neutralize the vacancy. Similarly, SnO2 releases some
oxygen, resulting in a different composition, initially SnO2-x Reflectance (R) is the ratio of the flux of reflected energy to the
(Vo")x e2x'. In general, the thin film sample is estimated to be incoming energy flux.
𝐼𝑛2−𝑦 𝑆𝑛𝑦 ′𝑂3−𝑥 (𝑉0 ")𝑥 𝑒2𝑥 ′𝑒𝑦 ′ , with 𝑆𝑛𝑦 ′ substitution Sn for (𝑛2 − 1)2 + 𝑘 2
In, which produces one free electron. 𝑅= (7)
(𝑛2 + 1)2 + 𝑘 2
The oxidation conditions result in a change in the The transmittance (T) of thin films can be determined by,
concentration of oxygen vacancies, which in turn can lead to 2𝑛1
𝑇=| | (8)
changes in carrier density. An increase in oxygen content in 𝑛2 +𝑛1
the ITO layer can also improve the orientation of carrier The relationship between the absorption coefficient (α) and the
mobility. On the other hand, the oxygen content may cause a extinction coefficient (k) can be expressed by,
change in carrier density without resulting in significant 4𝜋𝑘
𝛼= (9)
changes in carrier mobility. The effect of increased oxygen 𝜆
density at the insertion site on grain boundaries and oxides is The absorption coefficient (α), the extinction coefficient (k), and the
wavelength (λ) are related, and the transmittance of electrons
not visible.
undergoing a direct transition can be described mathematically.
Changes in the density and mobility of the carriers are 𝑛
𝛼 ℎ 𝑣 ≈ (ℎ 𝑣 − 𝐸𝑔 ) (10)
caused by several processes during annealing, including
With Eg representing the bandgap of the transition energy band, the
oxygen absorption and diffusion in the thin films. The
photon energy, and n = 1/2 for the direct transition and n = 3/2 for the
diffusion of oxygen can lead to a decrease in oxygen
indirect transition.
vacancies. Annealing may cause the diffusion of Sn impurity
atoms from grain boundaries and insertion lattice sites to
normal lattice sites, allowing Sn to act as an active donor due
to its atomic valence being greater than that of In. This
annealing process improves the crystallinity or crystal
growth, thereby minimizing scattering between the grain
 as shown in Fig. 7. The energy bandgap changes because the
concentration of Sn doping atoms begins to decrease due to the
bonding of Sn atoms with oxygen introduced from the outside. As a
result, the electron wave functions at the impurity level no longer
overlap, affecting the potential energy level changes of each electron,
which may lead to the formation of an energy band in the region.
Another effect that arises from the reduced concentration of
impurities is the expansion of the lower energy band, which causes
the bandgap energy to undergo a tailing band effect.
The shift in the energy band gap can also be associated with the
annealing temperature, which is related to the atom diffusion rate of
oxygen at the grain boundary. An increase in partial oxygen pressure
Figure 7. Band gap energy ITO. may lead to an increase in transmittance, as shown in Fig. 8, resulting
The transmission changes with partial oxygen pressure and from changes in the crystallization of the ITO thin layer, with FWHM
annealing levels, as shown in Fig. 8. increasing as shown in Fig. 4. ITO-coated grains begin to transition
from the amorphous structure to fine grains with sizes ranging from
68.99 nm to 122.76 nm at temperatures between 150°C and 250°C.
The changing pattern of ITO layer transmittance in response to
partial oxygen pressure and annealing changes is shown in Fig. 8.
The high transmittance observed in some samples up to a certain
range appears to correspond to the properties of the ITO material,
which has a wide energy band gap ranging from 3.78 eV to 4.35 eV.
The shift in the energy band gap due to vacancies was formulated by
Burstein-Moss [33].
𝐸𝑔𝑓𝑓 = 𝐸𝑔0 + ∆Ʃ𝑔𝐵𝑀 + ħ Ʃ (𝑘)
Where the contribution of electron scattering is due to impurities. To
reduce the contribution of electron impurities from In and Sn, the
Figure 8. ITO Transmittance. addition of partial pressure oxygen causes a decrease in electron
The change in the bandgap of the ITO coating energy is impurities, resulting in an increase in the energy band gap [34].
influenced by changes in partial oxygen pressure and annealing,
Table 3. Optical parameters of ITO thin films for
different oxygen partial pressures and annealing conditions.
Oxygen Wave Absorption Maximum
Annaeling Ref Refractive Attenuation
Partial Length Coefficient Transmittance
(oC) (%) Index Constant (k)
(a) (%)
(%) (nm)
175 686 11.96 2.18 3.30 0.061 81.94
2.50
250 598 10.38 2.20 3.34 0.070 82.65
175 664 9.65 2.20 3.36 0.063 84.05
3.70
250 615 8.39 2.18 3.36 0.069 84.71
175 591 8.40 2.20 3.38 0.072 84.41
5.10
250 615 7.70 2.20 3.40 0.072 85.05
175 727 9.61 2.09 3.08 0.053 85.07
6.15
250 664 10.76 2.22 1.93 0.036 85.59
175 668 7.00 2.22 3.44 0.065 86.60
8.90
250 700 6.61 2.25 3.49 0.062 87.12
4. CONCLUSIONS

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