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Mediterranean Journal of Chemistry 2019, 7(6), 433-451

A review of nanostructured thin films for gas sensing and

corrosion protection
Ho Soonmin 1,* S. A. Vanalakar 2 , Ahmed Galal 3 and Vidya Nand Singh 4
1
Centre for Green Chemistry and Applied Chemistry, INTI International University, Putra Nilai, 71800,
Negeri Sembilan, Malaysia
2
Department of Physics, K. H. College, Gargoti, Tal- Bhudargad, Dist- Kolhapur, 416209, India
3
Chemistry Department, Faculty of Science, Cairo University, 12613, Giza, Egypt
4
CSIR-National Physical Laboratory, New Delhi, 110012, India

Abstract: Thin film technology is getting huge attention across the world due to its wide applications. Deposition
of thin films involves creation, transportation and condensation of target materials with thickness varying from
few nanometers to several microns onto the substrate. This review will highlight thin film depositing techniques
which consist of non-vacuum and vacuum based deposition method. Besides this, thin films and their applications
in gas sensing and corrosion protection have also been discussed.

Keywords: thin films; semiconductor; gas senor; deposition; corrosion protection.

Introduction (data storage 4), environmental (smart window 5),

energy (solar cells 6-10), heat prevention & corrosion
Thin Film Technology resistance (gas turbine components 11,12), and super
hard coatings 13. Thin film coating can be classified
Thin film technology has progressed rapidly in
according to coating thickness. Usually, researchers
the direction of thin film coating and also has been
have deposited films with thickness in the range of a
developed for the need of the industry. It serves a
few nanometers to 10 µm are considered thin-film
number of purposes for various uses, including
coatings. The thin films can have different properties
electronics (flexible polymer light-emitting displays 1,
compared to bulk material 14-16. Common processes in
optical coatings (anti-reflection coatings 2),
recent thin-film technology include vacuum based and
superconducting films (SQUID3), magnetic films
non-vacuum based technology as shown in Figure 1.

Vacuum based Non vacuum

technique based technique

Electro
Evaporation
deposition

Sol Gel
Sputtering
technique

Nanoparticle
Pulsed laser
based
deposition
technique
Figure1. Various thin film deposition techniques.

*Corresponding author: Ho Soonmin Received October 6, 2018

Email address : soonmin.ho@newinti.edu.my Accepted November 10, 2018
DOI: http://dx.doi.org/10.13171/mjc7618111916hs Published November 19, 2018
Mediterr.J.Chem., 2018, 7(6) H. Soonmin et al. 434

Various Deposition Techniques of applications from microelectronics to photovoltaic

cells. Here, evaporation, sputtering and pulsed laser
Various vacuum 17-20 and non-vacuum based
deposition were selected as shown in Figure 1.
techniques 21-24 have been used for depositing thin
films by various researchers across the globe. Evaporation
Researchers are using these techniques for depositing Evaporation is a well-known technique for
thin films for different applications. These methods depositing thin films for many applications. In this
are briefly discussed below. technique, the material is heated inside a high vacuum
chamber. Low vapor pressure is sufficient enough to
Vacuum Based Technique
raise a vapor cloud inside the chamber and deposit on
Vacuum-based techniques have been the standard to the substrate. The basic thermal evaporation
for high-quality semiconductor fabrication for a range schematic is shown in Figure 2.

Figure 2. Schematic of evaporation technique

Memarian and co-workers deposited nanostructured sputtering is to deposit insulating oxide films.
CdS thin film using thermal evaporation and study the Reactive sputtering is a process where the target is
effect of temperature (25 to 250 °C) on film 25 in a sputtered in the presence of a gas or a mixture of
vacuum of about 2X10-5 Torr. The resistivity values gasses (e.g. Ar + O2) which reacts with the target
observed (3.11 to 2.2 X 104 .cm) depend on the material to form a coating of a different chemical
substrate temperature. Daniel and co-workers studied compositions.
Cu3SbS3 thin films deposited by evaporation for solar
Singh and co-workers deposited petal type
energy harvesting application 26. Jung and co-workers
structure of Cu2ZnSnS4 (CZTS) using reactive
fabricated copper indium gallium selenide (CIGS)
sputtering 31. Siol and other workers demonstrated
thin film solar cells using evaporation and study the
reactive sputtering of In2S3 as an alternative contact
effect of Ga content on properties of absorber material
27 layer for CZTS thin film solar cells from the single
. Steinmann and co-workers demonstrated tin
target in the presence of 98 % argon and 2 % H2S gas
sulfide solar cell with 3.88 % efficiency by using
mixture 32. Gour and co-workers deposited CZTS thin
evaporation 28. Xu and co-workers studied
film using DC sputtering and studied the effect of
microstructure and properties of ZrC-SiC multi-phase
sodium on properties of deposited thin films 33. In
coatings prepared by thermal evaporation where ZrC-
another study, CuIn and CuGa were deposited on a
SiC coatings have a multi-layered structure with low
glass substrate using DC sputtering followed by post
silicon (Si) content, and a single ZrCx-SiC layer with
selenization for CIGS thin-film solar cell applications
high Si content 29. 34
. Gorjanc and other workers deposited indium tin
oxide (ITO) thin film on a glass substrate using radio
Sputtering
frequency (RF) sputtering at room temperature having
Sputtering is a process whereby coating material
transparency between 70-90 % in the visible range,
is dislodged and ejected from the solid surface in the
and the sheet resistance was about 18 Ω.cm 35. Choi
form of atoms/molecules due to the momentum
and other workers studied the effect of oxygen
exchange associated with surface bombardment by
concentration on properties of Zn(O,S) thin film
energetic particles. This phenomenon is known as
deposited using RF sputtering 36. Gour and other
sputtering, as shown in figure 3. McClanahan and co-
workers studied the effect of NaF on properties of the
workers have presented a historical review of sputter
Cu2ZnSnSe4 thin film deposited using RF sputtering
deposition 30. DC (direct current) sputtering is used to
from in-house made single target for solar cell
deposit metallic films where RF (radio frequency)
applications 37.
Mediterr.J.Chem., 2018, 7(6) H. Soonmin et al. 435

Figure 3. Schematic of the sputtering phenomenon.

In another study, Cu2ZnSn(S, Se)4 thin film based performance of CZTS based photodetector for visible
photodetector for visible range were fabricated using to NIR range 45.
RF reactive sputtering 38. Obeng and other workers
deposited molybdenum sulfide (MoS2) thin film using Pulsed Laser Deposition (PLD)
reactive sputtering 39. Gour and other workers Pulsed laser deposition (PLD) has been used to
demonstrated rice-like nanostructured (rln) CZTS thin deposit high-quality thin films of materials. In this
film based self-powered broadband photodetector technique, high power laser pulses (about ~108
deposited on a glass substrate using reactive Wcm-2) were used to strike to a material that is to be
sputtering 40. Gour and other workers prepared DC deposited onto the substrate. The melted, evaporated
magnetron-sputtered Zn(O, S) films on a quartz and ionized material from the surface of a target
substrate and studied the effect of sulfurization comes from the target in the form of plasma. The
temperature on optical, morphological, elemental and ablated material is collected on a suitably placed
structural properties 41. Gour and other workers substrate upon which it condenses, and the thin film
studied the effect of Ag incorporation on properties of grows on to the substrate. Figure 4 shows the
reactively sputtered CZTS thin film for solar cell and schematic of the pulsed laser deposition technique.
other optoelectronic device applications 42. Huq and Zhao and co-workers deposited ZnO thin film on a
other workers deposited GaN thin film using RF silicon substrate where film deposited in no-oxygen
sputtering and studied the effects of surface disorders ambient at 500 ℃ used as a buffer layer for growth of
and incorporate on the thin films characteristics 43. ZnO thin films 46. Zeng and co-workers studied
Singh and other workers fabricated CZTS thin film substrate temperature dependent (300 to 700 °C) ZnO
solar cell having efficiency of 2.84 % using reactive thin films prepared on titanium substrate using PLD
sputtering on glass substrate 44. Singh and other for microwave, and medical applications 47.
workers studied the effect of sodium on the

Figure 4. Schematic of pulsed laser deposition technique.

Han and co-workers deposited cascade structure photocatalyst applications 49. Kotani and co-workers
of Bi2S3/CuInS2/TiO2 thin films using PLD technique studied compositional analysis of CZTS thin film
for high photoelectrochemical performance for the deposited on soda lime glass substrate 50.
direct fabrication of QD sensitized solar cells 48.
Yamaki and co-workers demonstrated epitaxial TiO2
films sapphire substrate by using PLD for
Mediterr.J.Chem., 2018, 7(6) H. Soonmin et al. 436

Non-Vacuum Based technique are connected to a potentiostat which is the instrument

which controls the deposition process. These
Cost-effectiveness is the core of the development
electrodes were kept within a container containing a
of any new technology. In this work, several non-
liquid which has ionic species dissolved within it,
vacuum methods such as electrodeposition, sol-gel,
such as copper ions dissolved in water. Rashid and co-
and nanoparticle-based technique have been chosen
workers deposited Cu2ZnSnS4 (CZTS) thin film
for the deposition of thin films based on various
grown on conducting glass substrate using a single
materials. These methods are briefly discussed below.
step by using electrodeposition technique and studied
the optical and structural properties51. Pawar and co-
Electrodeposition
workers deposited Cu2ZnSnS4 thin films for solar cell
Electrodeposition is considered one of the low-
application using electrodeposition technique on Mo
cost methods for the production of semiconductor thin
coated glass and ITO glass substrate and studied
films. Electrodeposition, also well-known as
structural, morphological, compositional, and optical
electroplating, is the technique in which material
properties 52. Jiang and co-workers demonstrated co-
deposited onto a conducting surface from a solution
electrodeposited Cu2ZnSnS4 thin film solar cell and
containing ionic species.
Cu2ZnSnS4 solar cell-BiVO4 tandem device for
This deposition technique is mostly used to unbiased solar water splitting application 53. Relekar
deposit thin films of material to the surface of an and co-workers studied effect of electrodeposition
object to change its external properties such as to potential on surface free energy and supercapacitance
increase corrosion protection, increase abrasion of MnO2 Thin Films prepared by electrodeposition
resistance, improve decorative quality, or simply to technique they observed specific capacitance (Cs) of
deposit a layer which is part of a more complicated MnO2 thin films is 127 F/g for the deposition potential
device. Schematic of electrodeposition is shown in at 1.20 V/Ag/AgCl and films also show better stability
figure 5. In this technique three electrodes are used for over 1000 cycles 54.
which are working, reference, and counter (sometimes
secondary) electrodes, respectively. The electrodes

Figure 5. Schematic of the electrodeposition technique.

Premnath and co-workers deposited Co1-xMoxS studied microstructural, corrosion properties and
thin films using electrodeposition technique on doped mechanical deformation response of deposited films
tin oxide (FTO) substrate which can be used as using high-resolution transmission electron
electrocatalysts for hydrogen evolution reaction (HER) microscopy, X-ray diffraction, electrochemical
in acid medium 55. Thomas and co-workers deposited workstation and triboindenter 58. Altiokka co-workers
silicon/rare earth (Er, Tb) thin films on n-doped deposited CdS thin films at various pH values using
silicon (100) substrate using single step electrodeposition. Compact CdS films with good
electrodeposition process and carried out crystallinity 59 were obtained at pH value of 4 and 5.
compositional, optical and microscopic analysis for Jiang and co-workers deposited graphene-Sb2Se3 thin
optoelectronic applications 56. Zhang co-workers films as photoelectrode using electrodeposition for
deposited nanocrystalline CoFe soft magnetic thin photoelectrochemical water splitting 60. Thorat and
films using electrodeposition technique from citrate- co-workers deposited nanocrystalline Bi2Te3 thin
stabilized baths 57. Xia and co-workers deposited Ni- films onto stainless steel substrates using
doped TiN thin films by jet electrodeposition and electrodeposition technique for photoelectrochemical
Mediterr.J.Chem., 2018, 7(6) H. Soonmin et al. 437

application. The photoconversion efficiency and fill Pingarron and co-workers demonstrated
factor of photoelectrochemical (PEC) cell made by electrochemical biosensor based on gold
Bi2Te3 film were 0.0987 % and 0.3979 %, nanoparticles 71. Hassan and co-workers demonstrated
respectively 61. Zhang and co-workers deposited thin a nanoparticle-based method for culture-free bacterial
NiFe hydroxide film as electrode for solar-to- DNA enrichment from whole blood 72. Hua and co-
chemical energy conversion 62. Devi and co-workers workers deposited multiple types of nanoparticle thin
deposited Fe–Ni–P thin films using electrodeposition films by lithographic technique 73. Sebastian and co-
and studied the effect of heat treatment on structural, workers deposited green silver-nanoparticle-based
optical and magnetic properties of deposited films 63. dual sensor where they examined the optical and
Mahato and co-workers deposited cadmium selenide electrochemical sensing behavior of silver
(CdSe) thin films on ITO coated glass substrates using nanoparticles from Agaricus bisporus (AgNP-AB) for
electrodeposition technique and studied the effect of toxic Hg(II) ions 74. Simonsen and co-workers
annealing on structural, optical and photosensitive demonstrated potential applications of magnetic
properties of deposited films. The photosensitivity of nanoparticles in the petroleum industry, and they
the CdSe film increased 64 upon annealing up to a observed that the adsorption capacities for
temperature of 350 °C. nanoparticles are around 90 % in case of water
separation from emulsions 75. Esfe and co-workers
Sol-gel Technique studied convective heat transfer and pressure drop of
The sol-gel process can be used for depositing aqua based TiO2 nanofluids of different diameters of
films on larger substrates. In the sol-gel process, the nanoparticles by data analysis and modeling with
liquid precursor is laid out onto the substrate, artificial neural network 76. Ashok and co-workers
followed by drying, and then firing. The operational deposited SnO2 nanoparticle for dye-sensitized solar
cost of the sol-gel process is low because the process cells applications and studied the electron transport
is very simple and does not need expensive equipment. characteristics of SnO2 nanoparticles 77. Georgiou and
Samarasekara and co-workers 65 studied structural co-workers made copper nanoparticle metal grids for
properties multilayered cupric oxide thin films cost-effective ITO-free solution processed solar cells
78
prepared by spin coating. Amin and co-workers and efficiency of 4.92 %. Nikam and co-workers
deposited magnesium doped gallium nitride thin films deposited CdSe nanoparticles on ZnO nanorods
by sol-gel and studied effects of the Mg concentration photoanode for solar cell application using successive
on the structural, surface morphology, elemental ionic layer adsorption and reaction (SILAR)
compositions, lattice vibrational and electrical technique at room temperature 79. Vijayakumar and
properties of deposited films 66. They found that by co-workers deposited vanadium carbide
increases Mg concentration, the resistivity of the thin nanoparticles-based counter electrode for dye-
films decreases while the hole concentration and hall sensitized solar cell 80.
mobility of thin films increases. Nebi and co-workers
deposited Co-doped TiO2 films using sol-gel Literature survey:
technique and estimated bandgap of deposited films 67.
Thin film technology in protection against
corrosion
Nanoparticle-Based Technique
Inks including dispersions of fine particles Protection of metals and alloys from corrosion is
present assured advantages over pure solution-based of prime interest for different industrial processes and
methods, including a broader selection of liquid applications. The necessity of protection against
vehicles, the possibility to use more compact corrosion has been driven from its costly damages.
precursors with close-to-targeted composition and Corrosion is a “reaction” that takes place between
minimal presence of foreign, chemically bound metallic structures and its surrounding environment.
species that have to be eliminated by thermal Mechanistically, this reaction can be physical,
processing and that have the potential to reduce the chemical or electrochemical. The most significant is
critical thickness of the layers (i.e. the maximum the electromechanical reaction, which involves the
thickness per layer that can produce a crack-free film). transfer of electrons between the reactants 81. Several
An early printing approach to deposit CZTS used approaches and techniques have been adopted for
particle-based (approx. 200 nm) precursors protection against corrosion. Those included oxide
synthesized by reacting metal salts with sulfur in hot film formations over metals and alloys 82, organic
ethylene glycol 68. Recently, a method was reported in inhibitors 83; different coatings approaches including
which component binary and ternary metal inorganic 84, polymeric 85, spray 86, chemical vapor
chalcogenide nanoparticles were used rather than the deposition 87, and anodization 88. Chromate and
multinary CZTS/Se particles to facilitate tailoring phosphate phases provide excellent corrosion
film composition, with efficiencies69 as high as 8.5 %. resistant coatings. However, they are restricted by
Prasad and co-workers demonstrated NH3 sensing environmental regulations in recent years 89 and are
properties of surface modified Ce-doped replaced with silicate, molybdate, rare earth, and
nanostructured ZnO thin films prepared by spray titanium oxides or zirconium oxides 90. Some
pyrolysis method 70. techniques adopted for applying thin films for
Mediterr.J.Chem., 2018, 7(6) H. Soonmin et al. 438

corrosion protection and their pertinent applications techniques have also been introduced such as sol-gel
are summarized in Table 1. technique 94, 95. Composite materials have several
properties that encouraged their use as coating
Recently, carefully designed coatings based on
materials which improve corrosion protection
thin-film technologies have been introduced 91.
efficiency. Among these properties: good adhesion
Coatings application to the surface of metals and
characteristics, strain tolerance, self-healing
alloys forms a physical or chemical barrier toward the 96
characteristics, and heat conductivity .
corroding environment. This is achieved by hindering
Environmental, economic, technical and societal
the migration of ionic species through the coating
factors encouraged the use of hybrid materials 97. The
layer, or when the coating act as a sacrificial anode, or
cost of the coating is another important issue for
embedding an inhibitor to the coating film 92..
consideration, therefore readily available materials
Specialty corrosion protecting coatings have been have been considered for film protection against
developed for advanced application such as aerospace corrosion 98, 99.
industries 93. In this respect, chemical and physical

Table 1. Some techniques used for thin films application and their applications in corrosion protection.
Techniques Applications
 Spraying Gas turbine components
 Thermal spraying Electrolytic cathode for copper refinement
 Chemical vapour deposition,  Water-cooled stator bars
 physical vapour deposition  Chips used in electrical generators
 Screen printing  Semiconductor device and the liquid crystal device
 dip coating
 thermal spraying
 Thermal spraying  Semiconductor processing equipment98
 Sputtering
 Immersion
 Chemical vapour deposition,
 physical vapour deposition

 Spraying immersion roll coating  Alkaline-containing environment

 Thermal spraying spray and fuse welding  High-temperature erosion-corrosion environments 99

Graphene has attracted extensive attention for its inhibition efficiency (IE) of 97.4 % is obtained by
unique properties including mechanical, chemical, protecting the underlying copper (Cu) against the
electrical among others, and has found several penetration of both dissolved oxygen and chlorine
advanced technical applications 100. Some of the ions. The increase of graphene coating thickness
recent applications of graphene are sensors 101, energy increased inhibition efficiency up to 99 %, which can
storage and conversion 102 and electronics 103. be attributed to the effective blocking of the ionic
Graphene offers spectacular properties being inert, diffusion process. Graphene was grown by chemical
lightweight, atomically thin, impermeable, wear vapor deposition over SUS304 stainless steel and on
resistant and mechanical strength that promotes its a catalyzing Ni/SUS304 double-layered structure 108.
application as a coating for corrosion protection 104. A 3.5 wt% saline polarization test demonstrated that
The inert role of graphene in a corrosive environment the corrosion currents in graphene-covered SUS304
showed new insight to develop anticorrosive coating were improved fivefold relative to the corrosion
layers on a metal substrate [24]. Due to its flexible and currents in non-graphene-covered SUS304. After a
transparent nature, graphene as a coating can tolerate corrosion test, the graphene-covered stainless steel
the curvature or roughness of the surface 105. exhibited not only an excellent low interfacial contact
resistance (ICR) of 36 mΩ cm2 but also outstanding
The basal plane of graphene offers chemical
drainage characteristics. Other reports described the
inertness and impermeability even to protons 106.
application of graphene as anti-corrosion and anti-
Acetone-derived graphene coating offered corrosion
oxidation coating on different substrates with
protection efficiency for copper in a seawater
different coatings 109-112.
environment up to 37.5 times higher as compared to
that of mechanically polished copper 107. Further, Another approach was introduced by the
investigation on the role of graphene coating on Cu formation of composite/hybrid structures of graphene
surfaces suggests that the outstanding corrosion and other materials for film formation over metal
Mediterr.J.Chem., 2018, 7(6) H. Soonmin et al. 439

substrates for protection against corrosion. Yang’s NiSO4, NiCl2, H3BO3 and WC powder (<1 m). The
group studied the fabrication of graphene reinforced solution pH was adjusted to 4.2, the temperature
waterborne polyurethane (PU) composite coatings on maintained at 50 ºC, and under stirring conditions, the
steel surfaces 113. applied current was 0.5 A cm-2 for 10 minutes. Ni-Co-
WC was also electrodeposited from a bath containing
Functionalization of these graphene composites
the same composition as for Ni-WC composition. The
with titanate was employed to facilitate the dispersion
microstructure developed between Ni-WC and Ni-
of graphene in the composite coatings. When the
Co-WC is a key factor in the development of dense
graphene content was 0.2 wt %, three-dimensional
and homogeneous surface resulting in hardness
random distribution of graphene was observed in the
improvement. The hardness of the coating layer
composite coatings, which gave an indirect path of
increased with the thickness. The Ni- WC coating
electrolyte to penetrate through the coatings. When
with 8 g/L NiCl2 in the electrodeposition bath realized
the graphene content reached 0.4 wt %, the graphene
the lowest corrosion rate for coated stainless steel in
layers were self-aligned parallel to the substrate
0.1 M H2SO4. In another study, nickel hydroxide-
surfaces. Graphene reinforced polyphenylene sulfide
graphene oxide composite coating was
(PPS) was reported that exhibited seven times higher
electrodeposited over 316-stainless steel by pulse
wear life than pure PPS coating 114. Graphene oxide
current method 122.
was synthesized by the Hummer’s method and then
functionalized to yield graphene. The as-produced A protection efficiency of 98.7 % against
solution was coated on steel substrates through spray corrosion was achieved in sodium hydroxide
coating. The major wear form was identified as containing solutions. The micro tribology
abrasive wear for graphene reinforced PPS coating measurements showed a decrease in the coefficient of
whilst the wear form of pure PPS coating was friction for the nickel hydroxide-graphene layer that
adhesive wear. was strongly adsorbed to the stainless steel substrate.
It was reported that the introduction of this layer
Graphene/pernigraniline composites (GPC) were
coating provided an increase in the friction on the
prepared by the in situ polymerization-
sample surface because of the rough surface provided
reduction/dedoping method. The synthesized
by the aggregation of Ni(OH)2 particles. Al2O3-SiC
composites have a flake-like structure, and their
reinforced Ni-matrix nano-composite coatings were
conductivity is as low as 2.3 × 10−7 Scm-1. The
deposited on steel and nickel substrates using a
composites possess not only impenetrable property
constant current of 1 Adm-2 at 45 ºC in Watts bath of
inherited from reduced graphene oxide but also
pH 4 for 60 minutes under stirring conditions 123. The
insulating property inherited from pernigraniline.
micro-hardness increased of the coatings increased in
Potentiodynamic polarization and electrochemical
the order Ni-Al2O3<Ni-SC<Ni-Al2O3-SC while the
impedance spectroscopy measurements revealed that
wear rate showed the opposite trend with the lowest
the GPC-modified coating is outstanding barriers
value reported for Ni-Al2O3-SC. The corrosion
against corrosive media compared with pernigraniline
resistance behavior of these coatings was studied in
or reduced GO modified films. Scratch tests also show
0.5 M Na2SO4 with the lowest corrosion current
that the corrosion-promotion effect of reduced GO in
density obtained, and optimum passivation behavior
GPCs is inhibited. Similar studies reported
was achieved when using the Ni-Al2O3-SC coating.
preparation of nano-clay reinforced polyaniline
The nucleation, growth mechanism and kinetics of
composites and their coatings on steel surfaces 115.
electrodeposited Ni-Co-SiC composite-coating on
The free-standing composite film exhibited a 400 %
carbon steel was studied by electrochemical
reduction in O2 permeability compared to
techniques and atomic force microscopy 124. Cyclic
conventional polyaniline, which in turn offered
voltammetry and open circuit potential measurements
significantly enhanced corrosion protection in the
indicated that Ni-Co-SiC requires more energy for its
form of composite coatings. Recently, other several
electrodeposition compared to Ni-Co coating. Atomic
studies reported the use of graphene composites as
force microscopy data showed that more nucleation
anti-corrosion coatings 116-119.
centers are formed for Ni-Co coating compared to Ni-
Nanomaterials can be used to protect materials Co-SiC formed after 2 seconds at -1.3 V (vs. SCE).
from tribocorrosion caused by simultaneous The results showed that more nucleation is reached as
mechanical and chemical/electrochemical the time of deposition increased and a uniform coating
interactions between surfaces in relative motion. is formed after 60 seconds deposition time. It was also
Nanomaterials such as FeCu/WC-Co and WC-Co, shown that the addition of SiC in the electrodeposition
electrodeposited Ni-Co alloy, Ni-nano SiC, bath decreased the efficiency of nucleation. The
electroless Ni-p-nano SiC coatings and authors indicated the formation of a clouding of inert
nanostructured titanium provide a lubricating effect particles around metal cations that increased the
that improves anti-trobocorrosion 120. Ni-WC energy of transport of these cations to the cathode
electrodeposition was achieved over stainless steel surface 124. It was also reported that the
electrodes from an organic-free Watt’s nickel chloride electrochemical driving energy controlled by the
in the presence of suspended ultrafine WC particles applied negative potential on the cathode overruled
121
. The Watts’ plating solution was composed of the role played by SiC particles at high cathodic
Mediterr.J.Chem., 2018, 7(6) H. Soonmin et al. 440

current densities. A new generation of thin coatings In this respect, nano-structured carriers are loaded to
are being developed and possess the property of self- the matrix of the coatings with different
healing based on inclusions that respond to different configurations to inhibit corrosion 125, 126.
stimuli such as pH, humidity or mechanical stresses.
Meso-porous oxides core is introduced as the using PVD technique, the method is relatively costly
basis for the preparation of nano-containers 127. and time-consuming.
The approach is based on a layer-by-layer Pulsed laser deposition (PLD) can also be used
assembly of oppositely charged species that prevented for the deposition of thin-films over metallic
the self-release of the corrosion inhibitor to the substrates for corrosion protection. The method relies
electrolyte. The burst of the nano-container shell was on the usage of short and highly energetic pulses to
induced by changing the pH value surrounding it, evaporate specific target particles that subsequently
which in turn is in response to the nature of corrosion condense over the desired substrate. Some studies
medium exposed to the coating 128. Nanotechnology- reported the use of PLD for depositing films such as
based self-healing coatings have also been corrosion protection of stainless steel using PLD of
successfully introduced for corrosion protection of thin films of Y2O3 136. The study showed good
metals and alloys 129. Self-healing approaches include protection of the Yttria layer to the steel substrate
corrosion conversion coatings, silane, sol-gel coatings when exposed to molten uranium and actinide wastes.
with nano-reservoirs and conducting polymers. In another study, the parametric conditions of the PLD
process were studied for the deposition of alumina
Thin films materials can also be deposited on
over stainless steel substrate 137. The results showed
metallic surfaces using several techniques for
that average mass removal rate on laser fluency,
different applications. Some of the commonly used
ablation geometry and average deposition efficiency
methods are chemical vapor deposition (CVD),
during PLD affected the structural and mechanical
plasma enhanced CVD (PECVD), physical vapor
properties of alumina thin film formation over the
deposition (PVD), pulse laser deposition (PLD),
steel substrate. The resulting α-alumina showed high
sputtering techniques and sol-gel methods.
corrosion resistance towards exposure to molten
Chemical vapor deposition for corrosion control uranium up to a temperature of 1165 C. The PLD
has been discussed in a recent review 130. The most technique faces some challenges such as the granular
commonly used PVD techniques are vacuum (by formation of thin film deposits that results in surface
evaporation), sputter and arc vapour depositions. The defects for corrosion protection application. For
coating resulting by PVD methods is hard but not example, iron thin films deposited by PLD on silicon
completely uniform due to defects developed such as wafer resulted in the corrosion of the film when
pores formation and columnar growth. The formed exposed to NaCl solution 138. In this study, optical
channels underneath the PVD coating allowed microscopy measurements showed localized
exposure of the underlying metal to the attacking corrosion at the peripherals of the particles within the
electrolyte to diffuse in. For example, the Ti2N film iron film matrix. Therefore, PLD technique can be
deposited over NdFeB resulted in the formation of useful in the application for thin film deposition for
pinholes and craters 131. It is possible to control the corrosion protection in targeted purposes but still
quality of the resulting deposited film using PVD faces the challenge of high cost and the development
technique by adjusting the operational parameters. of surface defects of some cases.
For example, the effect of the bias voltage of the
A chemical synthesis process based on sol-gel
substrate on the protection ability of chromium
was also used successfully to deposit thin films over
carbide film over AISI D2 steel was studied 132. The
metallic substrates for corrosion protection 139. The
authors found that the protection ability increased
ultimate product formed by the sol-gel method is the
when the bias voltage decreased as indicated by the
formation of an oxide network through a chain
lowering in corrosion potential. It was also reported
condensation reaction of an inorganic metallic
that the bias voltage used over the substrate decreased
precursor 140. Generally, a metal or metalloid alkoxide
the corrosion resistance of the metal by developing a
in the form of M(OR)n is an organic solvent is used as
porous film of TiCN and TiNbCN on AISI 4140 133.
a precursor where M is Si, Ti, Al, Zr, Fe, etc. Sol-gel
In general, PVD coatings are vulnerable to aggressive
thin films were formed over a variety of surfaces for
attacks in chloride containing electrolytes. Surface
corrosion protection such as steels, stainless steel,
defects developed from PVD deposition of thin films
aluminum, aluminum alloys, copper, magnesium,
can be remediated by multilayers coatings. In this
magnesium alloys, etc. The formed layer resulted in
respect, a multilayer coating of Ti/TiN was
the formation of either of the following: metal oxide,
investigated; the study showed enhancement in
organic/inorganic hybrid sol/gel, inhibitor-doped
corrosion resistance for the coated steel in different
sol/gel and inorganic-metal sacrificing coatings. Si-,
electrolytes 134. In another study, a double coating of
Zr-, Al-based oxides and alike possess high chemical
Al2O2/Al/Ti over steel compared to AlTiO2Ti or Al/Ti
stability that allowed good protection for the
provided better corrosion resistance for steel in NaCl
corresponding substrates in acidic media and under
solution 135. While double coating strategies could be
high-temperature operations 141. Organic/inorganic
effective in reducing the formation of surface defects
hybrid sol-gel coatings suffered from some drawbacks
Mediterr.J.Chem., 2018, 7(6) H. Soonmin et al. 441

including cracks developed from rather thicker layers UV/visible light, the magneto-resistive sensors based
and the necessity of applying relatively higher on the change in resistivity due to the presence of an
temperature to cure the formed films 142. Sol-gel layer external magnetic field. The chemo-resistive sensors
could also be impregnated with an inhibitor to measure the change in the resistivity produced by the
synergistically overcome corrosive medium for the interaction of a chemical substance with the sensing
metallic substrate. The strategy, in this case, depends material 150. However, among various gas sensors, a
on the incorporation of an organic inhibitor 143 or chemo-resistive thin film based gas sensors are
inorganic-based inhibitor. The addition of cerium promising because of the low cost and relative ease of
acetate into the sol-gel layer reduced the amount of operation, short response time, long life time, simple
unreacted water-soluble silane and formed a passive control electronics and highly sensitive to all ranges
ceria based film that resisted the chloride attack to the of the gases. However, relatively low sensitivity and
metal substrate. poor specific selectivity, sensitive to the
environmental factor and high operating temperatures
An alternative approach using sol-gel method is
are some of the drawbacks of the chemo-resistive gas
to coat the substrate with inorganic metal-rich
sensors 151. The materials utilized in these sensors are
(sacrificed) coatings. The sacrificed metals such as
as often as possible prepared in thin film form, and
zinc or magnesium were included in the sol-gel layer.
they can be synthesized by various physical and
This resulted in cathodic protection of the underlying
chemical methods.
metal substrate. Three coatings strategies have been
adopted including post-cured, self-cured and self- In the chemoresistive type of gas sensors, the
cured approaches based on water-based alkali metallic metal oxides are the most suitable materials. The gas
silicates and solvent-based alkyl silicates, sensing process by a metal oxide involves two key
respectively 144. A hybrid sol-gel impregnated with functions such as identification of a target gas through
Mg primers was developed 145. In this study, the a gas–solid interaction. The gas-solid interaction
coatings were sacrificed as a protecting element for induces an electronic change of the oxide surface and
aluminum alloys in 0.1% NaCl. However, in dilute followed by the transduction of the surface
Harrison solution, the rate of corrosion of the phenomenon into an electrical resistance change of
magnesium embedded in the sol-gel layer was the sensor 152. However, the complex nature of the
relatively higher compared to the NaCl solution. semiconducting oxide surface, including, porous,
polycrystalline sensing bodies comprising nano-sized
Thin film based gas sensors grains, the understanding of gas-solid interaction is
not straightforward. Historically, Seiyama and co-
Thin film based gas sensors are promising
workers 153 was the inventors of gas detection by metal
transducers used to detect a variety of oxidizing and
oxide thin films. Soon after the work of Seiyama,
reducing gases. This type of sensors is made up of
Tagushi fabricated the first commercial gas sensor.
various sensing elements in thin film form over a non-
Since then a large number of gas sensors were
conducting substrates such as soda lime glass. The
developed and fabricated using various materials
change in physical-chemical, optical and electrical
including metal oxides, chalcogenides, polymers,
properties of thin film materials in the presence of gas
graphite 154. The commonly used metal oxides to
is the basic principle used to detect the various gases.
fabricate gas sensors including, SnO2, ZnO, In2O3,
The thin film gas sensors mainly consist of photo-
WO3, Fe2O3, Ga2O3, Cr2O3, TiO2, V2O5, HfO2,
resistive, thermo-resistive, piezo-resistive, magneto-
CdIn2O4, SrTiO3, and Li2SnO3 155-160. Fig. 6 and Table
resistive and chemo-resistive materials as a sensor
2 show the number of publications on ‘Thin Film Gas
element 146-150. In the thermo-resistive sensors, the
Sensors’ from 1998 through mid-2018 (Source:
resistivity variation is controlled by the temperature,
Scopus Data). Fig. 6 and Table 2 show that the gradual
whereas piezo-resistive sensors use the change in
increase in the publications was observed during the
resistance with mechanical stress. The photo-resistive
stated period.
sensors show sensing properties in the presence of
Mediterr.J.Chem., 2018, 7(6) H. Soonmin et al. 442

Year of publication Number of publication

1998 205
1999 188
2000 193
2001 205
2002 195
2003 257
2004 266
2005 383
2006 314
2007 315
2008 368
2009 320
2010 336
2011 382
2012 393
2013 411
2014 438
2015 380
2016 463
2017 392
2018 378
Figure. 6. Number of publications based on ‘Thin Film Gas Sensor’ from 1998 to mid of 2018 (Source: Scopus
data).
Table 2. Number of publications based on “Thin Film Gas Sensor” from 1998 to 2018. (Source: Scopus data).

The important aspects of thin film gas sensors are phenomenon. In particular, the oxygen-related defects
a substrate, sensing elements, contacts, temperature or vacancies induce a large number of electron
and controller, chamber design, etc. As stated above, donor on the surface of metal oxides 163. As a result of
the most important sensing element are metal oxide defects, a large number of electrons may capture from
semiconductors. There are two types of metal oxide the conduction band of metal oxides to form a thicker
semiconductors such as transition and non-transition electron depletion layer, which suggests the better
type. The transition type metal oxide semiconductor response of the sensor. In addition to the defect
contains more oxidation states as compared to its concentration, the operating temperature plays an
closest counterpart. The oxidation states are important role in the gas sensing properties of metal
influencing factor on the requirement of the energy 161. oxide thin film sensors. The metal oxide thin film
Therefore, transition-metal oxides are most often sensors reported a higher sensitivity at the high
utilized as sensing elements, compared to the non- working temperature. The possible reason is the
transition metal oxides. Also, transition-metal oxides higher reaction O− species at an elevated temperature.
with d0 (such as WO3, TiO2, V2O5) and d10 (such as In the fabrication of a thin film gas sensor, the sensor
ZnO, SnO2) electronic configurations are commonly element layer has to be preheated to the desired
reported as sensing element 162. temperature using micro-hotplate or filaments. At the
higher working temperature, the probability of gas
Additionally, the n-type metal oxide
molecule adsorption is increased on the metal oxide
semiconductors are preferable in sensing research as
layer surface. The ohmic contact is another factor
compare to p-type semiconductors, even though they
influencing the gas performance of thin film gas
require a relatively lower operating temperature.
sensors. The ohmic contact is a metal-semiconductor
Several other influencing factors, such as the nature
contact having negligible resistance. Particularly, the
of the surface, the structure of the sensing layer,
electric contacts with the sensing material should be
defects, size affect the sensing properties of metal
ohmic. In general, the contacts should not interact
oxides as a gas sensing element. The gas sensing
with gas, and there should not be diffusion into the
phenomenon is mainly a surface dependent activity;
sensing material.
therefore, a higher surface area leads to the higher
sensitivity of the thin film gas sensors. Therefore, The progress of thin film gas sensors is acceptable
nanosized thin film structure is a more suitable for technological reasons. It is possible to prepare gas
candidate than the bulk films. Also, the presence of sensing devices with low power consumption and
the defects plays an important role in the gas sensing small size which can easily be integrated into an array.
Mediterr.J.Chem., 2018, 7(6) H. Soonmin et al. 443

Metal oxide semiconductors are the most studied volume ratio, therefore, they were not widely used to
sensing elements in thin film based gas sensors and fabricate thin film gas sensors. On the other hand, the
showed the most satisfactory characteristics for gas chemical or solution based deposition methods such
detection. However, an extensive research effort as chemical bath deposition (CBD), electrochemical,
should require to improve the knowledge of working sol-gel, spin coating, spray pyrolysis, hydro-
mechanisms of thin film gas sensor and their long- solvothermal methods are appropriate to produce
term stability. porous and nanostructured thin films, which are well
suitable for gas sensing applications. Also, chemical
Thin film gas sensors were prepared via various
methods give numerous surface morphologies to
physical and chemical synthetic routes. Also, a
enhance surface-to-volume ratio. Less sophisticated
combination of physical and chemical method,
experimental setups, low-cost equipment, no need of
another method is known as hybrid techniques, such
vacuum and requirement of lower temperatures for
as plasma deposition and reactive evaporation also
the depositions are additional advantages of chemical
have been reported to deposit a thin film gas sensor in
methods over the physical methods 170.
the literature. Generally, in any synthesis method,
three basic steps took place such as the creation of Electro-chemical deposition technique is well
ions, transportation through suitable medium and known solution based method used to coat metal
condensation on the substrate. Among various oxides over the substrate with various morphologies.
physical thin film deposition method, thermal It requires an external source of current and
evaporation is relatively simple and convenient conducting substrate for the deposition. In literature,
technique. In this technique, the target material very meager work is found on the electro-deposited
vaporizes after heating to a suitable temperature. Then thin film gas sensors. Meanwhile, the chemical
the vapour condensate onto a cooler substrate which solution deposition techniques are extensively used to
forms thin solid films. However, the evaporated films fabricate thin film gas sensors. The easy to engineer
are not uniform. The non-uniform film thickness the surface morphology, shape, porosity, surface area
occurs because the amount of the target material to volume ratio, the formation of defects via chemical
reaching the substrate depends on the angle between methods harmonically results into the better sensing
the source and the substrate surface 164. It is well properties. Spray Pyrolysis, CBD and Sol-gel
known that better quality thin films can be deposited techniques are the most popular among chemical
by sputtering technique. Therefore, the number of solution-based deposition methods. In the spray
publications on the deposition of thin film for gas pyrolysis technique, an oxide thin film will have
sensor using sputtering are higher than evaporation formed when a metallic salt solution is sprayed onto a
technique. However, non-porous film formation by hot substrate. The doped and mixed thin films can be
sputtering method restricts its wide applications for prepared very easily by using the spray pyrolysis
sensing purposes. Along with evaporation and method.
sputtering techniques, a high vacuum method such as
Meanwhile, the CBD technique is mainly used for
epitaxial deposition, laser deposition methods also
chalcogenide films. Recently, CBD has been extended
used to prepare thin film based gas sensors 165. The
to the deposition of metal oxide thin films. The CBD
deposition of mono-layer by mono-layer is carried by
method is comprehensively used to fabricate thin film
epitaxial methods, but, the nanostructured and porous
based gas sensors to detect various toxicants.
layer formation is difficult to achieve 166.
However, the formation of the undesirable precipitate
Meanwhile, chemical vapour deposition (CVD) is in the bulk of the solution is the main drawback of the
also a promising, versatile and flexible physical CBD method. In order to avoid such precipitation, a
technique to deposit good quality thin films. The CVD CBD is modified (which is also known as successive
method offers a simple set-up, the requirement of low- ionic layer adsorption and reaction, SILAR or
vacuum, easy to dope the impurities, etc. Therefore, modified CBD (MCBD)). Recently, few reports were
about 50 research articles were published on CVD found on the formation of gas sensor deposited via
deposited thin film gas sensors. However, the SILAR technique. It has been reported that the
complex reaction kinetics, high substrate temperature, performance of thin film gas sensors is improved by
difficulty in masking the substrate are some of the using chemical methods. In general, the chemical
drawbacks of CVD. methods are the most appropriate techniques to
deposit nanostructured and porous films. Also, doping
The ease in commercial mass production,
is easy, and defects can be easily found in the
possibility to deposit controlled stoichiometric
chemically deposited film. All the factors are
compounds, relatively pure products are the
responsible for better sensing performance.
advantages of the physical techniques 167, 168. Though,
the gas sensing performance governed by the In addition to the deposition techniques, the
diffusion of gas through the pores of the sensing nanostructure plays a very important role in the
layers which can be enhanced by engineering the performance of thin film based gas sensors. Nano-
surface properties such as porosity, shape, surface materials has already demonstrated a range of
area to volume ratio 169. The physical techniques are highly sensitive and selective gas sensor designed for
not suitable to produce porosity, higher surface-to- very low-power operation. In addition, the
Mediterr.J.Chem., 2018, 7(6) H. Soonmin et al. 444

nanostructured gas sensors can detect multiple gases representation of nanostructured thin film gas sensors
simultaneously. The research on multiple gas used to detect various gases.
detection is undergoing. Meanwhile, Fig. 7 shows the

Figure 7. FESEM images of (a) PVP/AMT before calcinations (the inset shows the corresponding high
magnification image); (b,c,d) WO3 nanofibers after calcinations and (e) response and recovery characteristics of
WO3 based gas sensor to different gases 171, (f to i) a carbon materials-functionalized tin oxide nanoparticles-based
sensing platform exhibits a highly selective response/recovery nitrogen dioxide behavior at a low working
temperature of 140 °C with a low limit detection of 2 ppm 172, (f and g) enlarged TEM image of SnO2/C core-shell
nanospheres, (h and i) schematic of sensing mechanism diagram of SnO 2/C core-shell nanospheres-based sensor
towards NO2, and (j) XRD patterns of nanostructured SnO2/rGO precursors and (k) Response versus operating
temperature (150–300 °C) of the SnO2 based sensors to 100 ppm ethanol (permission is taken from Elsevier) 173.

Conclusion:
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