Journal of 3D Printing and Applications

ISSN: 2831-8846
DOI: 10.14302/issn.2831-8846.j3dpa-22-4066

Review Article Freely Available Online

Thin Film Deposition and Characterization Techniques

Temesgen Geremew1,*

1Debark University, Department of physics, Debark, Ethiopia

Corresponding author:
techniques contains sputtering deposition, electron
Temesgen Geremew, Debark University,
beam evaporation and physical vapour deposition
Department of physics, Debark, Ethiopia. Orcid
(PVD) process have been known for over 100 years
ID: https://orcid.org/0000-0002-5144-9508
and also fabrication films on the substrate, as well as
Keywords:
the increasement of the pressure in the chamber due
Physical Methods, Chemical Methods, Thin Films, to operation of the sources indicates directly that
Chemical Bath Deposition, Characterization of Thin gases or vapors are desorbed. Chemical deposition
Films, Physical Vapour Deposition process is economically effective and has been
Received: Jan 15, 2022 industrially exploited to large scale. It can be
summarized that thin film characterization
Accepted: Apr 05, 2022
techniques include X-ray diffraction (XRD), UV-Vis
Published: Apr 07, 2022
spectrophotometer, scanning electron microscopy,
Abstract energy dispersive x-ray diffraction, transmission
Thin films are everywhere in the modern electron microscopy (TEM). X-rays diffraction (XRD)
world, with many of the technologies we depend is a rapid and a powerful technique used to study the
upon in daily life being, in turn, dependent upon phase of a crystalline material, information on unit
thin film technology. Chemical bath deposition cell lattice parameters, crystal structure, crystal
includes principles of chemical bath deposition orientation and crystalline size.
(CBD) and concept of solubility product, Introduction
nucleation and film growth, thin film deposition
Thin-film deposition processes for solid-state
mechanism in chemical bath deposition. The
device fabrication are needed in many steps in the
non-metallic ion source (anions) and metal ion
fabrication process. It is important that compatible
source (cations) then react to form the compound.
deposition processes are selected that do not
The nucleation process plays an important interfere with the structures already built into the
role in determining the crystallinity and device. The process integration, which has to
microstructure of the resultant film. consider thermal effects, chemical and metallurgical
From the discussion of deposition compatibility as well as functional requirements and
techniques which are physical and chemical limitations, is a major consideration in successful
deposition methods. Physical deposition process selection. Frequently, the deposition

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processes have to offer a high degree of flexibility in In Physical deposition techniques, such as, physical vapor
meeting the demands for specific device requirements. deposition, electron beam’s evaporation and thermal
The process selection has to be based on adjusting evaporation techniques. In this technique, physical
deposition parameters such as film thickness, uniformity deposition method of the deposition processed through
and composition [1]. Thin film deposition is the physically can’t take place chemical reaction. However, in
technology of applying a very thin film of material chemical deposition techniques contains just like that of
between a few nanometers to about 100 micrometers, or chemical vapour deposition, successive ionic layer
the thickness of a few atoms onto a "substrate” surface to adsorption and reaction (SILAR) and chemical bath
be coated, or onto a previously deposited coating to form deposition. In chemical deposition techniques which have
layers. Thin film deposition manufacturing processes are been used ultrathin film growth. In addition, in chemical
at the heart of today’s semiconductor industry, solar deposition method chemical reaction takes place but in
panels, disk drives, and optical devices industries [2]. physical deposition method doesn’t take place chemical

Thin films are everywhere in the modern world, reaction. In case of chemical deposition techniques is to

with many of the technologies we depend upon in daily produce high quality films.

life being, in turn, dependent upon thin film technology. Physical Deposition Techniques
These may range in dimension from an atomic or Physical Vapor Deposition (PVD)
molecular monolayer—perhaps only a few angstroms
The main aspects of the physical vapour
thick—to either mono- or multilayer coatings with a thick-
deposition methods are compiled in Figure 1. Preparation
ness of several microns. Such materials may have a huge
of the films takes place in a vacuum chamber
range of extremely useful properties; they may be, for ex-
characterized by the residual pressure (in the range of
ample, anti-reflective, impervious to oxygen and/
10-3 – 10-9 Pa) and by the composition and partial vapors
orothergases, optically transparently electrically
( in high vacuum (HV) range water vapor, oxygen,
conductive, catalytic, and self-cleaning. Everyday
nitrogen and hydrocarbons, in the ultrahigh vacuum range
examples featuring thin film technology include, but are
(UHV) mainly CO, H and He). The vaporized species of the
not limited to, mobile phones, touch screens, laptops, and
film material components are produced mainly by
tablets [3, 4]. Other important applications of thin films
evaporation or sputter source(s) [15]. The characteristics
include band pass filters as used in gas analysis [5],
of the emitted species are the flux J, energy E, sizes (atoms,
mirrors used in astronomy [6–8], protective (e.g.,
clusters) and ionization state (neutrals or ions) which
biomedical, anticorrosive, and antimicrobial) coatings [9],
depend on the material(s) and on the type and working
architectural glass coatings (e.g., to reflect heat while
parameters of the source. The kinetic energy, E, of species
transmitting visible light) [10], photovoltaic electricity
is 100-200 MeV at thermal evaporation and 5 to 10 eV of
generation [11,12], and a great many others.
sputtered species at floating substrate potential. This last
In the present time, thin films can be fabricated in one is in the order of, or larger than the bonding energy in
various ways. The techniques can be divided into physical solids. The transport of free species emitted by the
methods (Top-down approach) and chemical (Bottom-up sources to the substrate makes possible to manipulate
approach) methods as described in Table 1 [13, 14]. their electrical charge and kinetic energy. However
The purpose of this review paper is to study species of the desorbed or residual atmospheric gases/
deposition techniques of thin film, factor influencing vapours and the products of the possible interactions
deposition process, thin film characterization and its between the source and the material have to be also
application. Distinguishing feature between physical considered. An increase of the pressure in the chamber
deposition technique and chemical deposition technique. due to operation of the sources indicates directly that

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Table 1. Classification of thin film deposition techniques

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gases or vapors are desorbed. This phenomenon has to be effective and has been industrially exploited to large scale.
considered carefully, because one part of these species Chemical Vapour Deposition (CVD)
impinge directly on the substrate and participate in the
Chemical Vapor Deposition (CVD) methods
structure evolution as unintentional impurities
where the films are formed by chemical reaction
(contaminants).
between incoming species on the substrate. The gas and
By this way the concentration of contaminant liquid source are included in this method such as CVD
species in the condensing vapor beam might be more (and varieties plasma-enhanced chemical vapor
significant than could be estimated from the total pressure deposition (PECVD), plasma assisted chemical vapor
measured in some part of the system [16], [17]. Most of deposition (PACVD), metal-organo chemical vapor
these contaminants operate as inhibitors, [18], [19] and deposition (MOCVD), low pressure chemical vapor
might have a remarkable effect both on the structure and deposition (LPCVD)), spray, electrodeposition, chemical
properties even at low concentration. Bath, dip coating; sol gel …etc.
Electron Beam Evaporation Additionally, it requires expensive high
Electron beam evaporation with subsequent temperature reaction furnace and/or vacuum
vacuum condensation of metals and nonmetals [20, 21]. environment, and expensive high vapor pressure
This method is technologically simple, provides rather compounds. A schematic diagram involving the steps in
high coating growth rates (up to several micrometers per the process of CVD is illustrated in Figure 2 according
minute), and allows a wide range of process to [25].
parameters [22]. In this method the material is In chemical vapor deposition (CVD) the
bombarded and heated by an electron beam. The electrons compounds of a vapor phase, often diluted with an inert
are accelerated by 2-6 KV to get high energy. A magnetic carrier gas, react at a hot surface to deposit a solid film
field is also applied to focus and bends the electron [26, 27]. The importance of CVD is due to the
trajectory. versatility for depositing a large variety of elements and
Thermal Evaporation Technique compounds at relatively low temperatures and at

One of the oldest techniques used for depositing atmospheric pressure. Amorphous, polycrystalline,

thin films is thermal evaporation or vacuum evaporation epitaxial, and uniaxially oriented polycrystalline films can

and it is widely used in the laboratory and in industry for be deposited with a high degree of purity. Aspects of CVD

depositing metal and metal alloys [23]. Thermal include the chemical reactions involved, the

evaporation deals with the evaporation of the source thermodynamics and kinetics of the reactors, and the

materials in a vacuum chamber and condensing the transport of material and energy to and from the reaction

evaporated particles on a substrate. This process is site.

conventionally called vacuum deposition. In this The following is a list of examples of some of the
technique, the material can be evaporated either by the common types of chemical reaction used in CVD.
heat generated by the resistance of a metal Pyrolysis
container [24]. The possible problems that can be
The simplest CVD process is pyrolysis, in which a
encountered in this technique are the source of material to
gaseous compound decomposes on a hot surface to
be vaporized and its purity.
deposit a stable residue. Examples are the following:
Chemical Deposition Techniques deposition of pyrolytic graphite from methane (CH4),
The chemical deposition process is economically which takes place at a substrate temperature of 22000C;

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 Figure 1. Main aspects of the physical vapour deposition

Figure 2. Schematic representation of CVD processes

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deposition of silicon from monosilane (SiH4), which takes gallium arsenide from the hot source at temperature T1 to
place in the range 800–13500C; and deposition of nickel the cooler substrate at temperature T2 through an
from carbonyl from [Ni(CO)4], which takes place at about intermediate gas phase of different chemical composition.
1000C [28]. Spray Pyrolysis
Reduction In this process the reagents are dissolved in a
Hydrogen is the most commonly used reducing carrier liquid, which is sprayed onto a hot surface in the
agent. Examples are deposition of silicon by the form of tiny droplets. On reaching the hot surface the
hydrogen reduction of silicon tetrachloride, which takes solvent evaporates and the remaining components react,
place at about 10000C, and deposition of tungsten by the forming the desired material. An example is the formation
hydrogen reduction of tungsten hexafluoride, which takes of cadmium sulfide films by spray pyrolysis of cadmium
place at about 8000C. Hydrogen reduction is also used to chloride and thiourea dissolved in water with the
accelerate the pyrolytic process by removal of unwanted substrate at about 3000C [29]. Table 2 shows many
byproducts as gaseous hydrogen compounds, for which applications of CVD processes.
less energy is required. Physicochemical Bases
Oxidation At the CVD process gaseous chemical compounds,
Silicon dioxide films can be deposited by the often diluted with an inert carrier gas, react on hot
reaction of silane with oxygen. surfaces in the reactor to form solid films, Fig. 3. The CVD

Nitridation process can be subdivided as follows:

Silicon nitride films can be deposited by reaction Production of a reaction gas mixture,

of silane with ammonia. Transportation phase, Deposition and film formation.

Carbidization The relatively high gas pressure is characteristic

in the transportation phase. It can amount to between
Titanium carbide films can be deposited by
10mbar and 10bar. The mean free path is small in
reaction to titanium tetrachloride with methane at a
relation to the dimensions of the recipient and/or the
substrate temperature of 18500C.
distance source – substrate d. CVD processes occur at
Chemical-Transport Reaction
small Knudsen numbers Kn
For these processes, the transport of the desired
(2)
material from the source to the substrate on which it is to
The high process pressure distinguishes CVD
form a film depends on the difference in equilibrium
from PVD. Because of the collisions in the gaseous phase
constants between the reactant source and carrier phase,
of the CVD process, the molecules, which create the film
and the substrate and the carrier phase, when each are
structure, must be sluggish in reaction, so that no
held at different temperatures. For example, the
powder developed in the gaseous phase and no
deposition of gallium arsenide by the chloride process
damaging secondary reactions take place. This means that
depends on the reversible reaction
as original substances not atoms, like in the PVD process,
but molecules that are sluggish in reaction must be used.
(1) An ideal characteristic curve for a thermal CVD process is

Where T1 is the temperature of the solid GaAs shown in Fig. 3.

source, T2 is the temperature of the solid GaAs substrate, At low temperatures (range I) the deposition
and T1 > T2. This allows, in effect, indirect distillation of process is determined by the reactions taking place at the

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Table 2. Application of CVD processes

Thin Film Application

Epi-Si Semiconductor material
a-Si Solar cells
Ge Tunnel diodes, solar cells
SiC Protective against oxidation
BN Diffusion source, crucible material
BP Photovoltaics
AIN Dielectric, piezoelectric material for acoustic wave beam
AIP Electroluminescent diodes
AlAs Electroluminescent diodes, solar cells
AlSb Solar cells
GaN Electroluminescent diodes
GaP Electroluminescent diodes
ZnSe Photoconductor, laser diodes
ZnTe Electro-optical applications
CdS Photoconductors, laser diodes, solar cells, detectors
CdS1-xSex Lasers
Zn1-xCdxS Lasers
Cd1-xHgxTe Photoconductors, laser, photo diodes
Pb1-xSnxTe Photoconductors, laser, photo diodes
Pb1-xSnxSe Lasers
PbS Photoconductors, lasers
PbTe Infrared detectors
PbS1-x Sex Lasers
PbSe Lasers
PbO Photoconductors
SiO2; PSG; BSG; ASG Passivation, etching mask, gate dielectric in MOS structures
Si3N4 Diffusions masks, oxidation masks, anti-reflection coating in solar cells
GaAs Semiconductor material
Gasb Laser diodes
InP Gun diodes, laser diodes
InAs Laser diodes, Hall effect diodes
InSb Photo electrodes
GaAs1-x Px High temperature rectifiers, electroluminescent diodes, laser diodes
InAs1-x Px Photo cathodes, electro-optical applications
InAs1-xSbx Laser diodes
GaAs1-xSbx Laser diodes, photo cathodes
Ga1-xInxAs Laser diodes, photo cathodes
Ga1-xInxP Luminescent diodes
Ga1-xAlxAs Laser diodes, solar cells
InxAl1-xP Electroluminescent diodes, laser diodes
W Metallization, conductive path in integrated circuits
Mo Schottky diodes, conductive path
Ta Conductive path

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surface. The deposition is described by Arrhenius law: gaseous phase occurs. With simple forms, e.g., coating of

(3) plane surfaces, other aspects are of importance. Thus, for

example, the desired film structure requires a defined
operating point. This is valid, for example, in the case of
Where the E the activation energy and R the
the Si epitaxy [30, 31]. At the silicon surface silane
universal gas constant. At higher temperatures the
decomposes according to the chemical equation
reaction rates at the surface become so fast that the
(4)
deposition is

Fig.3. with the chemical the vapor deposition, e.g.,

Moreover, the silicon growth rate is
of metals, a precursor molecule at a temperature T1
proportional to the partial pressure of silane. For
reacts with hydrogen (H2) to a complex, which deposits
cases where the reaction is surface controlled, epitaxial
itself to the coated surface. At the substantially higher
growth proceeds according to the following steps: Mass
temperature T2 of the substrate the complex decomposes
transfer of the reactant molecules (SiH4) by diffusion from
into an organic remainder of R and a metal atom, which
the turbulent film across the boundary film to the silicon
forms the nucleus for layer growth with others
surface.
Fig.4. Ideal CVD characteristics curve, I the
1. Adsorption of the reactant atoms on the surface.
deposition process is determined by the reactions taking
place at the surface, II determined by the flow in the 2. The reaction of a series of reactions that occur on the

reactor and approximated temperature- independently, III surface.

homogeneous reactions in the gaseous phase 3. Desorption of the byproduct molecules.

Determined by the transport through the gaseous 4. Mass transfer of the byproduct molecules by diffusion
phase. In this range the deposition rate and the uniformity through the boundary film to the main gas stream.
of the film is determined by the flow in the reactor and 5. Lattice arrangement of the adsorbed silicon atoms.
approximated temperature independently (range II). At
The overall deposition rate is determined by the
still higher temperatures (range III) the deposition is
slowest process in the list above. Under steady- state
controlled by homogeneous reactions in the gaseous
conditions all steps occur at the same rate and the
phase, which can finally lead to powder formation. The
epitaxial film grows uniformly. Depending upon
deposition rate is thereby reduced. Figure 5 shows the
deposition conditions different reactor types is used. For
different types of characteristic curves. The selection of
the kinetically controlled range (range I) batch reactors
the operating point on the CVD characteristic curve de-
are suitable. The flux plays a subordinated role in this case
pends on:
only. Due to low eluviation’s larger numbers of work
1. The form of the work pieces pieces can be coated at the same time. In the range II the
2. The film structure. deposition is strongly affected by the flux, however higher

Fig.5 Different types of CVD characteristics coating rates are to be expected.

curves, (1) suitable for batch reactor, (3) for high Successive Ionic Layer Adsorption and Reaction (SILAR)
deposition rates SILAR is aqueous solution technique based on
If complicated forms or porous work pieces are to sequential reactions at the substrate solution interface for
be coated on the inside, then the operating point is always the deposition of thin films. The SILAR was developed by
selected within the kinetically controlled range, because Nicolau for the deposition of zinc and cadmium
of the low deposition rate at which no eluviation of the chalcogenides thin films [32]. The adsorption is a surface

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Figure 3. with the chemical the vapor deposition, e.g., of metals, a precursor molecule at a temperature T1
reacts with hydrogen (H2) to a complex, which deposits itself to the coated surface. At the substantially
higher temperature T2 of the substrate the complex decomposes into an organic remainder of R and a
metal atom, which forms the nucleus for layer growth with others

Figure 4. Ideal CVD characteristics curve, I the deposition process is determined by the
reactions taking place at the surface, II determined by the flow in the reactor and approximated
temperature- independently, III homogeneous reactions in the gaseous phase

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phenomenon between ions and surface of substrate and is monly used because it is a very simple, cost effective and
possible due to attraction force between ions in the economically reproducible technique that can be
solution and surface of the substrate. These forces may be applied in large area deposition at low temperature.
cohesive forces or Van der Waals forces or chemical Chemical bath deposition is used to deposit thin films of a
attractive forces. Atoms or molecules of substrate surface wide-range of materials. The deposition mechanism is
possess unbalanced or residual force and hold the largely the same for all such materials. A soluble salt of the
substrate particles. Rinsing follows each reaction, which required metal is dissolved in an aqueous solution to
enables heterogeneous reaction between the solid phase release cations. The non-metallic element is provided by a
and the solvated ions in the solution [33]. In spite of its suitable source compound which decomposes in the
simplicity, SILAR has a number of advantages. It is presence of hydroxide ions, releasing the anions. The
relatively inexpensive, simple and convenient for large anions and cations then react to form the compound. This
area deposition. technique is based on the controlled release of metal ion

In principle, it is possible to deposit metal (M 2+) and sulphide (S 2−) or selenide (Se 2−) ions in an

chalcogenide thin films using this method on to variety of aqueous bath in which the substrates are immersed. In

substrates [34]. The starting materials are commonly this process, release of metal ion (M 2+) is controlled by

available and cheap. As it is a chemical method, a large using a suitable complexing agent [39]. The solubility

number of varieties of substrates can be coated. Thus, any product gives the solubility of a sparingly soluble ionic salt

insoluble surface to which the solution has free access will (this includes salts normally termed insoluble). Sparingly

be a suitable substrate for the deposition. soluble salt CD, when placed in water, a saturated solution
containing C + and D− ions in contact with undissolved
Figure 6 represents the deposition of thin film
solid CD is obtained and equilibrium established between
using SILAR method. It consists of four different steps
the solid phase and in the solution as
such as adsorption, rinsing (a and b), reaction and rinsing
(c and d) [33]. (5)

Chemical Bath Deposition

Chemical bath deposition (CBD) method is most Applying law of mass action

commonly used because it is a very simple, cost effective (6)

and economically reproducible technique that can be
applied in large area deposition at low temperature.
Where K solubility [C+],[D-] and [CD] are
Chemical bath deposition is used to deposit thin films of a
concentrations of C+, D- in the solution, respectively. The
wide-range of materials [36]. The deposition mechanism
concentration of pure solid is a constant number i.e.
is largely the same for all such materials. A soluble salt of
the required metal is dissolved in an aqueous solution, to
release cations. The non-metallic element is provided by a
suitable source compound, which decomposes in the
presence of hydroxide ions, releasing the anions. The
anions and cations then react to form the compound [37].
(7) (8) (9)
In addition, the experimental set up of CBD techniques
described in Figure 7 below. Since K and K* are constants of KK*is also constant, say
Ks,therefore Eq.
Principles of Chemical Bath Deposition (CBD) and
Concept of Solubility Product CBD method is most com- (10)

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 Figure 5. Different types of CVD characteristics curves, (1) suitable for batch reactor,
(3) for high deposition rates

Figure 6. Schematic representation of SILAR method (a) cationic precursor and (c) anionic precur-
sor and (b, d) deionised water [35].

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 The constant KS is called solubility product (SP) The formation of solid MmXn is based on the
and [C+][D−] is called ionic product (IP). When the solution principle that when the ion product, [Mn+][Xm−], exceeds
is saturated the ionic product is equal to the solubility the solubility product, Ksp, of MmXn, then MmXn can form
product. When the ionic product exceeds the solubility as a solid phase, although a larger ionic product may be
product (IP/SP = S>1), the solution is supersaturated required if super saturation occurs. If the ion product does
(where S is degree of super saturation), precipitation not exceed Ksp, no solid phase will form, except possibly
occurs and ions combine on the substrate and in the transiently due to local fluctuations in the solution, and
solution to form nuclei [40]. the small solid nuclei will redissolve before growing to a

Nucleation and Film Growth stable size. For that reason, the precipitation process is an
equilibrium rather than as a one-way reaction.
Growth of thin films, as all phase transformation,
involves the process of nucleation and growth on the Simple Cluster (Hydroxide) Mechanism

substrate or growth surface. The nucleation process plays In most of the CBD’s, the preparative conditions
an important role in determining the crystallinity and are chosen so that the formation of metal hydroxide
microstructure of the resultant film. For the deposition of should be avoided. However, in reality, CBD’s are quite
thin films with thickness in the nanometer region, the often carried out under conditions where a metal
initial nucleation process is even more important. The size hydroxide (or hydrated oxide) is formed. This might seem
and shape of the initial nuclei are assumed to be solely to imply that a precipitate of metal hydroxide [M (OH)n] is
dependent on the change of Gibbs free energy, due to formed at the start of the CBD. In fact, the metal hydroxide
supersaturation, and on the combined effect of surface and formed is either as a colloid (rather than a precipitate) or
interface energies governed by Young's equations [41]. as an adsorbed species on the substrate but not in the bulk

Thin Film Deposition Mechanism in Chemical Bath of the solution. In this case metal chalcogenide (MmXn) is

Deposition formed by reaction of Xm− ion with the M(OH)n.

There are four main mechanisms leading to (12)

compound formation, whose operation depends on the Followed by

specific process and reaction parameters. The thin film (13)
growth in CBD occurs via the following four possible
The deposition of the thin film takes place
mechanisms.
through the condensation of the metal and sulphide/
1. Simple Ion-by-Ion Mechanism selenide ions on this initial layer which acts as a catalytic
2. Simple Cluster (Hydroxide) Mechanism surface.

3. Complex-Decomposition Ion-by-Ion Mechanism Complex-Decomposition Ion-by-Ion Mechanism

4. Complex-Decomposition Cluster Mechanism In this mechanism, complex at ion of free metal

Simple Ion-by-Ion Mechanism cations (Mn+) by chalcogenide source (thiourea,

thioacetamide) gives M-chalcogenide source complex ion.
In most of the CBD’s, the ion-by-ion conceptually
This is illustrated by the example of CdS deposition from
simplest mechanism, often assumed to be the operative
thiourea
one in general. It occurs by sequential ionic reactions. The
general reaction for the mechanism (14)

(11)
This ion is hydrolyzed by breaking the S-C bond to

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from CdS. thickness (\ 1 lm), possess higher surface energy due to its

(15) large surface to volume ratio; thus responsible for

different physical, material and chemical properties than
This would lead to CdS formation in solution. If
their bulk counterpart [42, 43]. This scope of tailoring
Cd2+ is adsorbed on the substrate (either directly or
materials’ to create the desired physical properties led to
indirectly through a hydroxide linkage) then above
large research activities in many areas such as
reaction occurs and CdS is formed on substrate, the result
microelectronics, optoelectronics, and sensors [44]. In
would be film growth by ion-by-ion. This mechanism is
these devices, precise growth of multiple layers of films
also useful in acidic solution; thioacetamide
(in either amorphous, polycrystalline or epitaxial form) of
decomposition at intermediate pH values, particularly in
polymers, metals, semiconductors, and insulators is
weakly acidic solution (pH ≥ 2) has been suggested to
essential to get the desired outcome. These films are
occur through a thioacetamide complex.
deposited using different techniques such as molecular
Complex-Decomposition Cluster Mechanism
beam epitaxy (MBE), chemical vapor deposition (CVD),
The complex-decomposition cluster mechanism is pulsed laser deposition (PLD), sputtering, thermal
based on the formation of solid phase, instead of reacting evaporation, e-beam evaporation, electroplating, and spin
directly with a free anion; it forms an intermediate com- coating techniques [42, 45].
plex with the anion-forming reagent. For CdS deposited
Thin film material properties do not always
from a thiourea bath the process can be described as:
resemble those measured at the bulk level. The
(16) application of thin films is becoming increasingly
interdisciplinary in nature, leading to new demands for
film characterization and properties measurements for
Cd(OH)2 is one molecule in the solid phase cluster.
both individual films and multilayer films [46].
This complex or a similar one if contains ammine ligands
then decomposes to CdS. Measurements and characterization of the film
thickness, micro-structure and composition can be carried
(17)
out using various techniques. They include X-ray
The S-C bond of the thiourea breaks, leaving the S
diffraction (XRD), UV-Vis spectrophotometer, scanning
bond to Cd. It is suggested that Cd(OH)2 forms initially on
electron microscopy, energy dispersive x-ray diffraction,
the substrate and catalyzes the thiourea decomposition.
transmission electron microscopy (TEM). In this review,
The catalytic effect of the solid surface could be to
we will use for structural analysis X-ray diffraction, for
decompose thiourea to sulphide ion and not necessarily to
optical analysis UV-Vis spectrometer and for
catalyze the complex- decomposition mechanism [38].
morphological analysis scanning electron microscopy.
Thin Film Characterization Techniques
X-ray Diffraction (XRD)
The thin-film characteristics are quite different
X-rays diffraction (XRD) is a rapid and a powerful
from the respective bulk counterparts. Materials, having at
technique used to study the phase of a crystalline material,
least one of the dimensions in the nanometer scale (less
information on unit cell lattice parameters, crystal
than 100 nm), are known as nanostructured materials,
structure, crystal orientation and crystalline size. XRD is
where properties are significantly different because of
widely used to characterize unknown crystalline
geometrical restrictions, causing novel physical and
materials. The working principle of the XRD technique is
chemical properties. Thin films (either it is polycrystalline,
relied on constructive interference of X-rays and a
or single crystal (epitaxial) or amorphous form) of a
crystalline sample. In a crystal, the atoms distribute

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regular in space, which comes into being crystal (19)
lattices [47]. The structural characterizations have
extensively used XRD, which is a non-destructive
If and only if this path difference is equal to any
technique. This technique can be used to determine the
integer value of the wave length
crystal structure of metals and alloys, minerals, inorganic
compounds, polymers and organic materials. A typical
XRD pattern consists of a series of peaks, in which peak (20)
intensity is plotted on the Y-axis and diffraction angle (2θ) In equating and , we have assumed that
along X- axis. These peaks are called reflections. The the angles of incidence equal the angles of reflection.
positions of the peaks in XRD pattern depend on the When the inter planar distance is denoted by d, it follows
crystal structure of the material while intensities depend from the Fig 8 that
on many factors like atomic structure factors, incident
(21) And
intensity, slit width, number of grains etc. [48]. X-rays are
(22)
a type of electromagnetic radiation with a wavelength
between 0.1 and 100 A exhibiting a high energy. In 1895
Wilhelm Conrad Rö ntgen first discovered X-rays and was From which it follow that

therefore awarded the Nobel Prize in Physics in 1901.

Hence, it is one of the most fundamental analytical (23)
techniques in research fields like solid state chemistry and
material science. In a common XRD setup, X-rays are (24)
generated in a high vacuum tube [49]. Bragg’s law
Putting everything together we get
expressed mathematically the crystal diffraction by
consider a crystal made of parallel crystals of ions, spaced
a distance d apart, and the constructive interference of (25)

the rays. By considering a crystal as made out of parallel Applying the trigonometric relation we get
crystals of ions, spaced a distance d apart Fig 8.

The conditions for a sharp peak in the intensity of the (26)

scattered radiation are: Which simplify to arrive at the following
1. That the X-rays should be secularly reflected by the condition for constructive interference:
ions in any one plane. (27)
2. The reflected rays from successive planes should
interfere constructively. Path difference between
Where n is the order of diffraction, λ the
consecutive rays reflected from adjoining crystal is
wavelength of the X-rays, d the distance of the lattice
rays is an integral multiple of the wavelength, That is
planes and θ is the Bragg angle and the glancing angle
(18)
between the incident beam and the reflecting crystals.
Where ∆d is the path difference and n = 1, 2, 3. Equation. (27) is known as Bragg’s Law. The possible 2θ

For the rays to interfere constructively, this path values where we can have reflections are determined by

difference must be an integral number of wavelength λ. the unit cell dimensions.

The path difference ∆d between rays 1 and 2 in the Fig (8) However, the intensities of the reflections are
is: determined by the distribution of the electrons in the unit

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Figure 7. Experimental set up of CBD technique [38]

Figure 8. X-ray diffraction from crystal.

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cell. The highest electron density is found around the surface of the samples then it systematically produces
atoms [50]. XRD measurement allows the calculation of large numbers of signals and these electron signals are
the distance of the lattice planes (d) in the crystal. The converted to a visual signal, which can be displayed on a
grain size of the crystallite is obtained by substituting screen [48].
values of Full Wave Half Maxi-mum (FWHM) in the The types of signals produced by an SEM include
well-known Debye- Scherrer formula is given by: secondary electrons; back scattered electrons (BSE), char-
(28) acteristic x-rays, light (cathodoluminescence), specimen
current and transmitted electrons. These types of signal
all require specialized detectors for their detection that
where D is grain size of the crystallite, K= 0.94,
are not usually all present on a single machine. When the
(λ=1.54059A ) is the wavelength of the Xray source used, β
beam of electrons strikes the surface of the specimen in-
is the broadening of the diffraction line measured at half
teracts with the atoms of the sample, signals in the form of
of its maximum intensity in radians (FWHM) and θ is the
secondary electrons, back scattered electrons and charac-
angle of diffraction at the peak [51].
teristics X-rays are generated that contain information
Scanning Electron Microscope (SEM)
about the samples, surface topography, composition, etc.
The scanning electron microscope (SEM) is one of The SEM can produce very high resolution images of the
the most promising technique for generating particle sample surface,revealing details about 1-5 nm in size in its
distribution profiles as well as surface characteristics with primary detection made i.e. Secondary electron imaging.
the possibility to visually reevaluate the data by Characteristics of X-rays are the second most common
re-assessing the particle. The technique holds promise for imaging mode for an SEM. These characteristic X-rays are
characterization of the size and shape of unknown prod- used to identify the elemental composition of the sample
ucts with relatively wide distribution profiles from the by a technique known as energy dispersive X-ray (EDX).
nanometer to the micron range [52]. Also very frequently, Back-scattered electrons (BSE) that come from the sample
scanning electron microscopes are equipped with may also be used to form an imaging. Back-scattered elec-
energy-dispersive X-ray (EDX) detectors, which are used tron images are often used in analytical SEM along with
for analyzing local elemental compositions in thin films. the spectra made from the characteristics X-rays as clubs
However, the possibilities of analysis in SEM go far beyond to the elemental composition of the sample [54]. The sche-
imaging and compositional analysis. It will be shown that matic image of SEM illustrated as:
imaging is divided into that making use of secondary elec-
UV/VIS Spectrophotometer (UV-VIS)
trons (SE) and of backscattered electrons (BSEs), resulting
Ultraviolet-visible spectroscopy (UV-VIS) is a
in different contrasts in the images and thus providing
spectroscopy (absorption or reflectance) in the ultraviolet
information on compositions, microstructures, and sur-
-visible region. The UV-VIS absorption spectroscopy
face potentials. Also, it will be demonstrated how im-
provides information of light absorption as a function of
portant it is to combine various techniques on identical
wavelength, which describes the electronic transitions
sample positions, in order to enhance the interpretation
occurring in the measured samples. The UV-VIS
of the results obtained from applying individual SEM
spectrophotometer detects the light intensity passing
techniques [53].
through a sample and compares the detected intensity to
SEM is one of the most important instruments
incident light intensity (light before passes through the
used for morphology analysis. The SEM generates images
sample). The absorbance A is simple expressed as Beer’s
by scanning the samples using a focused electron beam.
law:
The SEM utilizes a focused electron beam to scan across

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 Figure 9. Schematic image of SEM

Figure 10. Schematic of the relaxation of an inner-shell-

excited atom

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 (29) Energy Dispersive X-ray Spectroscopy (EDX or EDS)

Energy dispersive X-ray analysis is a technique to

Where the ratio is I/I0 called transmittance, I is analyze near the surface elements and estimate their

the intensity of light passing through the sample and I0 is proportion at different position, thus giving an overall

the intensity of light before passing through the mapping of the sample. This technique is used in

sample [55]. The optical band gap of materials is a very conjunction with SEM. The electron beam strikes a surface

important parameter that determines the application of of a conducting sample. The energy of the beam is

the films. It is evaluated using the stern relation formula: typically in the range 10-20 Kev. This causes X-rays to be
emitted from the material. The energy of the X-rays
emitted depends on the material under examination. The
(30)
X-rays are generated in the region about 2 microns in
Where α is absorption coefficient, A is the depth, and thus EDX is not truly a surface science
parameter which depends on the transition probability, technique [54]. Energy dispersive X-ray spectroscopy
ν the frequency of the incident beam, h is Planck’s (EDX) in the electron microscope has become an
constant and hv is the incident photon energy. For n =1/2, important tool for elemental analysis or chemical
2, 2/3, 3 allowed direct, allowed indirect, forbidden direct characterization for all types of solid material. The
and forbidden indirect transitions, respectively. For di- bombardment of a material with high energy electrons
rect band gap materials, n = 1/2, and n = 2, for indirect will result in the emission of characteristic X-rays, whose
band gap materials. The plot of α2 or (αhν)2 versus pho- wavelengths depend on the nature of the atoms in the
ton energy, hν (in electron volts) with extrapolation of the specimen. For the emission of the characteristic X-rays, an
straight line portion of the curve to zero absorption coeffi- atom has to be excited. There by an electron from an inner
cient (hν axis) gives the band gap energy for direct band shell will be knocked out. This state is instable and the
gap materials. The plot of α1/2 or (αhν)1/2 versus pho- empty state will be filled up from a more energy-rich
ton energy hν (in electron volts) with extrapolation to ze- electron from an outer shell.
ro absorption coefficient (hν axis) gives the band gap en-
Depending from which shell the more energy-rich
ergy for indirect band gap materials [51]. And also the
electron is coming and in which unoccupied inner shell
absorption band gap (Eg) has been calculated by using the
state it goes, the created X-rays are identified as Kα, Kβ
Tauc relation.
and Lα according from which shell the electron was
(31)
excited and from which shell the electron fills the empty
state. The wavelength of this X-ray can be calculated with

Where A is proportionality constant, h is the the following equation:

Planck’s constant, ν is the frequency of vibration, hν is the (32)

photon energy, α is the absorption coefficient and n is

either 2 for direct band transitions or 1/2 for indirect
Where h is the Planck constant, c the speed of
band transitions. The absorption coefficient (α) has been
light and ∆E the energy difference of the states involved
calculated using the relation α = 2.303A/t, where t is
[49].
thickness of the film and A is optical absorbance of film.
Transmission Electron Microscopy (TEM)
The direct band gap energy Eg estimated from a Tauc plot
of (αhν)2 versus photon energy hν. The value of photon Transmission electron microscopy is a good

energy (hν) extrapolated to α = 0 gives an absorption edge complementary technique to XRD for evaluating the

which corresponds to a band gap Eg [56]. crystallography of materials, and it is conventionally

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applied to obtain microstructure of materials using a the resolution of TEM Figure 11 [60].The principles of
high electron beam (≥ 2ookeV). TEM uses the electrons image formation in the TEM are the following (figure 11):
transmitted through a specimen illuminated with a (1) the focused electron beam impinge on the extremely
focused beam of electrons to form image, which is thin (30-60 nm) specimen, (2) the electron beam interacts
magnified and directed to appear either on a fluorescent with the specimen. This interaction results in the scatter-
screen or layer of photographic film, or to be detected by a ing of the transmitted electron beam. (3) The objective
sensor such as a charge-coupled device (CCD camera). The lens forms a diffraction pattern in the back focal plane
electrons are generated by thermionic or field emission with electrons scattered by the sample and combines
accelerated by an electrical field and focused onto the them to generate an image in the image plane (first inter-
sample using electrical and magnetic fields. A crystalline mediate image). Thus, diffraction pattern and image are
material interacts with the electron beam mostly by simultaneously present in TEM. In selected area diffrac-
diffraction rather than absorption, although the intensity tion mode (SAED), an aperture in the plane of the first
of the transmitted beam is still affected by the volume and intermediate image defines the region for which the dif-
density of the material through which it passes. The fraction is obtained (Figure 11). Which of them appears in
specially prepared sample is a very thin (less than 100 the plane of the second intermediate image and is magni-
nm) slice of material. The electrons pass through the sam- fied by the projective lens on the viewing screen depends
ple and the diffraction pattern and image are formed at on the intermediate lens. Switching from real space
the back focus plane and image plane of the objective lens. (image) to reciprocal space (diffraction pattern) is easily
If we take the back focus plane as the objective plane of achieved by changing the strength of the intermediate lens
the intermediate lens and projector lens, we will obtain [61].
the diffraction pattern on the screen. It is said that the When taking image (Figure 11), an objective
TEM works in diffraction mode. If we take the image plane aperture is inserted in the back focal plane of the
of the objective lens as the objective plane of the interme- objective lens to select one or more beams that contribute
diate lens and projector lens, we will form image on to the final image (BF, DF, and HRTEM). Including the
screen. It is the image mode. The resolution of the TEM direct beam into the objective aperture bright field
techniques is usually 0.3nm. In the most powerful diffrac- image is formed (BF), while selecting only scattered
tion contrast TEM instruments, crystal structure can also beams, dark field image (DF) can be received. Switching
investigated by high resolution transmission electron mi- from real space (image) to reciprocal space (diffraction
croscopy (HRTEM), also known as phase contrast imaging pattern) is easily achieved by changing the strength of the
as the images are formed due to difference in phase of intermediate lens [61].
electron waves scattered through a thin specimen. In
Conclusion
HRTEM images, contrast is not intuitively interpretable as
In this review, an overview of the deposition
the image is influenced by strong aberrations of the imag-
methods, thin film characterization and major deposition
ing lenses in the microscope. Resolution as high as 0.5 A
of thin films has been given. Films may be prepared by
has been obtained with HRTEM [57-59] HRTEM [57-59].
many different methods. However, these may usually be
Figure 9, Figure 10.
classified into chemical or physical methods. In the
The microstructure of thin films was investigated
physical methods the film is deposited from a vapour,
by transmission electron microscopy (TEM) using a
maintained at a pressure considerably below that of the
Philips CM20 microscope. In the transmission electron
atmosphere. Generally, there isn’t an exclusively chemical
microscopes monochromatic illumination (electron beam
bath deposition to produce thin films, but there is also
with energy from 100 KeV up to 1 MeV) is used to enhance

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 Figure 11. Schematic of a TEM [60], [61].

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chemical vapour deposition, thermal evaporation and Mauczokl, R.; Reimann, K.; Renders, C.; Roest, A.;
electron beam Evaporation to produce thin films. Roozeboom, F.; et al. Application of Dielectric,
However, in chemical methods the films is deposited from Ferroelectric and Piezoelectric Thin Film Devices in
a various chemical reactions to generate a vapour. In this Mobile Communication and Medical Systems. In
review which is briefly summarized characterization of Proceedings of the 15th IEEE International
thin films such as X-ray diffraction, Ultraviolet-visible Symposium on the Applications of Ferroelectrics,
spectroscopy (UV-VIS), Energy Dispersive X-ray Sunset Beach, NC, USA, 30 July–2 August 2006;
Spectroscopy (EDX or EDS) and Transmission electron Volume 2006,pp. 9–16. [CrossRef]
microscopy (TEM). The image seen with a transmission 5. Fleming, L.; Gibson, D.; Song, S.; Li, C.; Reid, S.
electron microscope (TEM) is formed by an electron beam Reducing N2O induced cross-talk in a NDIR CO2 gas
that passes through the specimen. A more recent and sensor for breath analysis using multilayer thin film
extremely useful investigative tool is the scanning electron optical interference coatings. Surf. Coat. Technol.
microscope (SEM). With optical microscopy, the light 2018, 336, 9–16. [CrossRef]
microscope is used to study the microstructure; optical
6. Birney, R.; Steinlechner, J.; Tornasi, Z.; MacFoy, S.;
and illumination systems are its basic elements. X-rays
Vine, D.; Bell, A.; Gibson, D.; Hough, J.; Rowan, S.;
diffraction (XRD) is a powerful nondestructive technique
Sortais, P.; et al. Amorphous Silicon with Extremely
for characterizing crystalline materials.
Low Absorption: Beating Thermal Noise in
Data Availability Gravitational Astronomy. Phys. Rev. Lett. 2018, 121,
The data that supports the findings of this study 191101. [CrossRef] [PubMed]
are available within the article. 7. S, tefanov, T.; Vardhan, H.; Maraka, R.; Meagher, P.;
Conflict of Interest Rice, J.; Sillekens, W.; Browne, D. Thin film metallic

The authors declare no conflict of interest. glass broad-spectrum mirror coatings for space
telescope applications. J. Non Cryst. Solids X 2020, 7,
Acknowledgement
100050. [CrossRef]
The authors would like to acknowledge Debark
8. Craig, K.; Steinlechner, J.; Murray, P.; Bell, A.; Birney,
and Addis Ababa University.
R.; Haughian, K.; Hough, J.; MacLaren, I.;Penn, S.; Reid,
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