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On Coating Techniques for Surface Protection: A Review
Article in Journal of Manufacturing and Materials Processing · March 2019

DOI: 10.3390/jmmp3010028
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Journal of
Manufacturing and
Materials Processing
Review
On Coating Techniques for Surface Protection:
A Review
Behzad Fotovvati 1, * , Navid Namdari 2 and Amir Dehghanghadikolaei 3
1 Department of Mechanical Engineering, The University of Memphis, Memphis, TN 38152, USA
2 Mechanical, Industrial and Manufacturing Engineering Department, The University of Toledo, Toledo,
OH 43606, USA; [email protected]
3 School of Mechanical, Industrial and Manufacturing Engineering, Oregon State University, Corvallis,
OR 97331, USA; [email protected]
* Correspondence: [email protected]

Received: 21 February 2019; Accepted: 18 March 2019; Published: 25 March 2019
Abstract: A wide variety of coating methods and materials are available for different coating
applications with a common purpose of protecting a part or structure exposed to mechanical or
chemical damage. A benefit of this protective function is to decrease manufacturing cost since
fabrication of new parts is not needed. Available coating materials include hard and stiff metallic
alloys, ceramics, bio-glasses, polymers, and engineered plastic materials, giving designers a variety
freedom of choices for durable protection. To date, numerous processes such as physical/chemical
vapor deposition, micro-arc oxidation, sol–gel, thermal spraying, and electrodeposition processes
have been introduced and investigated. Although each of these processes provides advantages, there
are always drawbacks limiting their application. However, there are many solutions to overcome
deficiencies of coating techniques by using the benefits of each process in a multi-method coating.
In this article, these coating methods are categorized, and compared. By developing more advanced
coating techniques and materials it is possible to enhance the qualities of protection in the future.
Keywords: surface modification; sol–gel; thermal spray; vapor deposition
1. Introduction
Mechanical parts and structures are designed for specific applications. Prior to fabricating these
parts, some extensive material selection constraints have to be met. These constraints include body
materials, mechanical properties (e.g., tension, compression, yield, torsion, fatigue, bending, and creep),
desired functionality (e.g., friction properties, hydrophobicity, wear resistance), thermal properties
(e.g., thermal expansion and conductivity to transfer heat flux), electrical conductivity, dynamic load
bearing (e.g., vibrations, high-speed rotation), and corrosion resistance. In addition, other parameters
such as availability, cost of materials, safety, and toxicity of these materials must be considered.
The latter category plays an important role in finalizing the material selection processes in advance to
manufacturing mechanical parts and structures. For instance, silver is known to offer high electrical
conductivity values, but fabricating a huge bulk of silver for electrical conductivity applications is too
costly [1]. NiTi alloys are well-known for showing the shape memory effect (SME) and superelasticity
(SE), which are useful in designing new actuators. Moreover, these alloys provide high biocompatibility
as they are used as bone implants that could be combined with SME, SE, or both, to develop new
biomedical devices for micro-surgeries inside the human body. However, the corrosion process of NiTi
in physiological environments releases Ni ions as byproducts, which are a toxic and harmful category
of materials for living organs [2]. Copper is a material with high thermal and electrical conductivity
with many applications such as brazing advanced materials; however, it suffers from low stiffness
J. Manuf. Mater. Process. 2019, 3, 28; doi:10.3390/jmmp3010028 www.mdpi.com/journal/jmmp

J. Manuf. Mater. Process. 2019, 3, 28 2 of 22
and wear resistance. In the case of copper rotary cooling fins, the durability of the mechanical parts
decreases significantly due to the high susceptibility of copper to wear mechanism [3]. To overcome
these issues and to enhance material properties for specific applications, there have been different
methods offered, such as heat treatment, alloying processes, and coatings. Among these solutions,
coating processes have the highest portion of material enhancement since coating layers can reduce
the cost and neglect scarcity of materials as the thickness of coating layers rarely pass micrometers.
This means less material is needed to form coating layers on a bulk of substrate materials. Coatings
can offer different properties such as corrosion/wear resistance, enhanced surface hardness, modified
surface texture, thermal/electrical insulation, enhanced wettability, hydrophobicity, etc. [4].
Coating methods are available in a wide variety due to the enormous diversity of applications
and needs in different fields. These processes consist of many different on-line/off-line parameters
while giving way to many different outcomes in the form of material microstructure, effectiveness,
suitability, and durability. However, coating methods are useful in specific applications according
to the desired functionality among which corrosion and wear protection are the most important [5].
Mechanical properties of the materials decrease by corrosion process whereas the corrosion products
are released in different forms that may cause a more extreme corrosive environment or harmful
side effects in different applications [6]. Coating materials have deferent deposition mechanisms
that needs to be investigated for the revelation of their pros and cons for the desired application.
There are many processes available, but only a few are among the most effective and applicable,
including physical vapor deposition (PVD), chemical vapor deposition (CVD), micro-arc oxidation
(MAO), sol–gel, thermal spray, and polymer coatings. Each of these methods is suitable for different
applications as they offer different deposition methods, different materials, second phases, different
thicknesses, and densities. As a result, mechanical stability, corrosion properties, biocompatibility (for
biomedical applications), and enhancement of material behavior for a specific type of coating have to
be considered carefully [7]. Although coating processes are applied to provide the abovementioned
benefits, they suffer from disadvantages that degrade their reliability. Of these adverse effects, negative
thermal effects (e.g., distortion, crack, delamination, etc.), destructive effects of loose atmospheric
protection (e.g., penetration of inclusions and contaminations into the substrate) and coating materials
properties (e.g., melting point, availability in different forms of foils/powders/rods, biocompatibility,
etc.,) are the most crucial ones to be considered.
Materials selection is the key parameter in having a successful coating as they provide all
protection purposes. Many different materials, including metals, ceramics, and polymers, can be
used to form a protective layer [8]. However, the diversity of coating processes and material properties
may cause difficulties in choosing the best composition of the deposited layer. To overcome this issue,
the most popular candidates such as Al, Ti, Hf, Zr, Ni, Co, Pt, MgO, ZrO2 , Al2 O3 , Y2 O3 , BeO, PEEK,
and PTFE must be considered while any probable new candidates should not be neglected. Although
each of the feedstock materials offer corrosion or wear resistance properties, they possess different
melting points, mechanical behavior, and chemical properties. Combined with their availability in
different forms of powders, rods, plates, and wires for specific uses, these parameters keep the material
selection in a narrower range. This review briefly covers common coating methods, materials, and
their surface modification quality whereas there are plenty of other protection processes such as heat
treatment, mechanical treatment, mechanical/chemical finishing, and polishing, which have not been
covered in this review.
2. Reliable Coating Methods

Coating processes provide protection to a specific part or area of a structure exposed to harsh and
corrosive environments in different fields ranging from aerospace and the automotive industry to tiny
biomedical devices and implants inside the human body.
more susceptible to a corrosive media. Figure 1 represents a schematic view of different types of
electron beam PVD machines. In this method, the coating growth is dominated by a physical
evaporation process. The thermal energy needed for evaporation may be supplied by different
supply units, such as electron beam, heating wire, laser beam, molecular beam, etc. [10]. This thermal
energy heats the atoms of the source material, which can be in the form of solid or liquid, to its
evaporation point. The vaporized atoms travel a distance through the vacuum and deposit onto the
substrate.
In different studies, the material composition of PVD coatings was investigated and they
2.1. Physical Vapor Deposition (PVD) Coating
claimed that the base material of the coating significantly affected corrosion properties of the coated
PVD process
parts. is famous
As an example, for offering
Mathew et al. corrosion and wear
[11] investigated theresistance
corrosion and thin protective
properties films on the
of two different
compositions
surface of single-layered
of the materials Ti-basedto(TiC
that are exposed xOy) and
corrosive Zr-based
media, and(ZrC Oy) coating layers.
its xapplications rangeThey
fromclaimed
decorative
that the Ti-based group provides better corrosion resistance compared to
objects to industrial parts [9]. The advantage of this method is that the mechanical, corrosion, the Zr-based, one and in and
the Ti-based group, the highest corrosion enhancement was provided by
aesthetic properties of the coating layers could be adjusted on demand. In general, PVD is a processsamples with 0.55–0.79
that fractions
takes place of oxygen in the coating composition. In other research related to the food industry by
in a high vacuum and the solid/liquid materials transfer to a vapor phase followed by
Damborenea et al. [10], the effect of the acidic environment of artificial casings in an acidic range of
a metal vapor condensation, which creates a solid and dense film. The most known types of PVD are
1–3 pH was investigated. They reported that the PVD coating of TiN on the surface of stainless-steel
sputtering and evaporation. Since the coating layers created by PVD are thin in nature, there is always
equipment increased corrosion resistance and protected the equipment from corrosion failure for a
a need for multilayered
significantly longer time.coatings while the
In addition materialsselection
to material selection forshould be considered
PVD coating carefully.
compositions, manyApart
fromresearchers
its decorative applications,
investigated many
the effect of PVD-coated parts
coating quality, serve as
porosity, andcomponents
adhesion onthat undergo
different a high rate
substrates
of wear that causes abrasion on the surface and removes the coating layer. This phenomenon
such as stainless steel, Ti-based alloys, and ceramics [12–15]. In summary, PVD coating can be utilized reduces
corrosion
in many resistance
applicationsproperties of the parts
such as aerospace, and makes
automotive, them more
biomedical susceptible
instruments, to and
optics, a corrosive
firearms.media.
It
provides
Figure the advantage
1 represents of flexibility
a schematic view ofindifferent
using anytypes
organic and inorganic
of electron beammaterial as a deposition
PVD machines. In thislayer
method,
while the
the coating coating
growth is layer offers high
dominated by a hardness
physical and corrosionprocess.
evaporation resistance The[16]. The PVD
thermal process
energy for for
needed
polymeric materials is challenging since the deposition leads to degradation
evaporation may be supplied by different supply units, such as electron beam, heating wire, laser of the polymer that
reduces the molecular weight of the film. PVD has been used for polyethylene (PE), polyvinylidene
beam, molecular beam, etc. [10]. This thermal energy heats the atoms of the source material, which
fluoride (PVDF), and conductive π-conjugated polymers such as poly(2,5-thienylene) (PTh), and
can be in the form of solid or liquid, to its evaporation point. The vaporized atoms travel a distance
poly(pyridine-2-5-diyl) (PPy) [17,18].
through the vacuum and deposit onto the substrate.
Figure 1. Schematic
Figure view
1. Schematic ofof
view a physical
a physicalvapor
vapor deposition (PVD)machine
deposition (PVD) machine using
using electron
electron beam
beam as the
as the
heat heat
source.
source.
In different studies, the material composition of PVD coatings was investigated and they claimed
that the base material of the coating significantly affected corrosion properties of the coated parts.
As an example, Mathew et al. [11] investigated the corrosion properties of two different compositions
of single-layered Ti-based (TiCx Oy ) and Zr-based (ZrCx Oy ) coating layers. They claimed that the
Ti-based group provides better corrosion resistance compared to the Zr-based, one and in the Ti-based
group, the highest corrosion enhancement was provided by samples with 0.55–0.79 fractions of oxygen
in the coating composition. In other research related to the food industry by Damborenea et al. [10],
the effect of the acidic environment of artificial casings in an acidic range of 1–3 pH was investigated.
They reported that the PVD coating of TiN on the surface of stainless-steel equipment increased
corrosion resistance and protected the equipment from corrosion failure for a significantly longer time.
In addition to material selection for PVD coating compositions, many researchers investigated the
effect of coating quality, porosity, and adhesion on different substrates such as stainless steel, Ti-based
alloys, and ceramics [12–15]. In summary, PVD coating can be utilized in many applications such
as aerospace, automotive, biomedical instruments, optics, and firearms. It provides the advantage
of flexibility in using any organic and inorganic material as a deposition layer while the coating
layer offers high hardness and corrosion resistance [16]. The PVD process for polymeric materials
is challenging since the deposition leads to degradation of the polymer that reduces the molecular
weight of the film. PVD has been used for polyethylene (PE), polyvinylidene fluoride (PVDF), and
conductive π-conjugated polymers such as poly(2,5-thienylene) (PTh), and poly(pyridine-2-5-diyl)

(PPy) [17,18].
J. Manuf. Mater. Process. 2019, 3, x FOR PEER REVIEW 4 of 21
2.2. Chemical Vapor Deposition (CVD) Coating
2.2. Chemical
Another Vapor
type Deposition
of vapor (CVD) Coating
deposition is called CVD. This process undergoes a high vacuum and
is widelyAnother
used intype
the semiconductors
of vapor depositionindustry
is calledproviding
CVD. This aprocess
solid, undergoes
high quality, andvacuum
a high a high and
resistance
is
widely used in the semiconductors industry providing a solid, high quality, and
coating layer on any substrate [19–22]. CVD can be used for mechanical parts in constant contact, a high resistance
whichcoating
need layer on anyagainst
protection substrate [19–22]. CVD
corrosion can beIn
and wear. used
thisfor mechanical
process, parts in constant
the substrate, knowncontact,
as a wafer,
which need protection against corrosion and wear. In this process, the substrate, known
would be exposed to a set of volatile material precursors where a chemical reaction creates a deposition as a wafer,
would be exposed to a set of volatile material precursors where a chemical reaction creates a
layer on the surface of the material. However, some byproducts of these chemical reactions, which are
deposition layer on the surface of the material. However, some byproducts of these chemical
removed by constant airflow of the vacuum pump, can remain in the chamber. A schematic of the
reactions, which are removed by constant airflow of the vacuum pump, can remain in the chamber.
CVD setup is shown in Figure 2. The vaporized CVD materials are pumped from the right side and
A schematic of the CVD setup is shown in Figure 2. The vaporized CVD materials are pumped from
the heaters keep
the right sidethe
andtemperature high the
the heaters keep enough to facilitate
temperature high the chemical
enough reaction
to facilitate thebetween
chemicalthe substrate
reaction
and vaporized materials.
between the substrate and vaporized materials.
Figure
Figure 2. Schematicchemical
2. Schematic chemicalvapor
vapor deposition
deposition (CVD)
(CVD) setup,
setup,mechanical
mechanicalparts, andand
parts, operation
operation
mechanism
mechanism [23].[23].
CVDCVD technique
technique providesaa wide
provides wideselection
selectionof of
materials in different
materials compositions
in different and forms
compositions andsuchforms
as carbides, nitrides, oxynitrides, a composition of Si with O and Ge,
such as carbides, nitrides, oxynitrides, a composition of Si with O and Ge, carbon in forms ofcarbon in forms of
fluorocarbons, diamond, polymers, graphene, fibers/nanofibers/nanotubes, Ti, and W. In addition,
fluorocarbons, diamond, polymers, graphene, fibers/nanofibers/nanotubes, Ti, and W. In addition,
these materials could be provided in different microstructures such as monocrystalline,
these materials could be provided in different microstructures such as monocrystalline, polycrystalline,
polycrystalline, and amorphous [24,25]. Moreover, CVD of polymers has been shown to be a reliable
and amorphous [24,25]. Moreover, CVD of polymers has been shown to be a reliable process in
process in applications such as biomedical device implants, circuit boards, and durable lubricious
applications suchCVD
coatings [26]. as biomedical deviceinimplants,
process performs circuit
three different boards, of
categories and durable lubricious
atmospheric coatings
pressure CVD, low- [26].
CVDpressure
process CVD,
performs in three different
and ultra-high vacuum categories
CVD, and the of atmospheric pressure
last two methods CVD,
are the mostlow-pressure
common onesCVD,
and [27].
ultra-high vacuum
There are many CVD, and the last two
other classifications methods
related are the
to the CVD most based
process common ones [27].
on substrate There are
heating,
many other classifications
material properties, andrelated to plasma
types of the CVD process
utilized in based on substrate
vaporizing heating,
the materials. material
These properties,
second-hand
categories
and types often include
of plasma utilizedaerosol-assisted
in vaporizingCVD, direct liquid
the materials. injection
These CVD, plasma-enhanced
second-hand categories often CVD,
include
microwave-plasma-assisted
aerosol-assisted CVD,
CVD, direct liquid hybrid physical-chemical
injection CVD, plasma-enhanced CVD, andCVD,photo-assisted CVD [28,29].
microwave-plasma-assisted
CVD, There arephysical-chemical
hybrid arguments on the CVD, advantages and disadvantages
and photo-assisted CVDof CVD There
[28,29]. over PVD based on the
are arguments on the
applications. In the CVD process, the substrate is heated up to 900 ℃, which cannot be used for
advantages and disadvantages of CVD over PVD based on the applications. In the CVD process,
temperature-sensitive materials. PVD provides a solution for materials of this kind. On the other
the substrate is heated up to 900 °C, which cannot be used for temperature-sensitive materials. PVD
hand, CVD has the advantage of less waste of materials since only the heated area can be coated. In
provides a solution for materials of this kind. On the other hand, CVD has the advantage of less
order to enhance this capability, computer-controlled lasers could be utilized to selectively heat the
waste of materials since only the heated area can be coated. In order to enhance this capability,
preferred areas [30,31].
computer-controlled lasers could be utilized to selectively heat the preferred areas [30,31].
2.3. Micro-Arc Oxidation (MAO) Coating
2.3. Micro-Arc Oxidation (MAO) Coating
MAO process is known as a flexible process of coating regarding the composition of coating
MAO The
layers. process is known
schematic of the as a flexible
process process
is illustrated in of coating
Figure 3. In regarding
general, MAOtheutilizes
composition of coating
a high voltage
difference
layers. betweenof
The schematic anode and cathode
the process to generate
is illustrated in micro-arcs
Figure 3. Inasgeneral,
plasma channels. Whenathese
MAO utilizes higharcs
voltage
hit the substrate, they melt a portion of the surface, depending on the intensity of
difference between anode and cathode to generate micro-arcs as plasma channels. When these arcs the micro-arcs. At hit
the same time, plasma channels release their pressure, which assists the deposition of coating
the substrate, they melt a portion of the surface, depending on the intensity of the micro-arcs. At the
sameJ. time,
Manuf. plasma channels
Mater. Process. 2019, 3, xrelease
FOR PEERtheir pressure, which assists the deposition of coating materials
REVIEW 5 of 21 in
the working electrolyte on the substrate surface. The existing oxygen inside the electrolyte causes a
materials
chemical reactionin the working electrolyte
of oxidation and provides on oxides
the substrate surface.
deposited on the The existing
surface oxygen
of the insidematerials.
substrate the
materials in the working electrolyte on the substrate surface. The existing oxygen inside the
electrolyte causes a chemical reaction of oxidation and provides oxides deposited on the surface of
The versatility of thisa process
electrolyte causes chemicallies in theofflexibility
reaction of combining
oxidation and desired
provides oxides elements
deposited andsurface
on the compoundsof
the substrate materials. The versatility of this process lies in the flexibility of combining desired
as a solute in the materials.
the substrate working electrolyte.
The versatility To of
date,
thisthe materials
process lies inmost commonly
the flexibility of coated with
combining MAO are
desired
elements and compounds as a solute in the working electrolyte. To date, the materials most
elements
Al, Mg, Ti, and andtheir
compounds
alloys [32].as aHigh
solutecorrosion
in the working
resistanceelectrolyte. To date,
is the most the materials
important most of
characteristic
commonly coated with MAO are Al, Mg, Ti, and their alloys [32]. High corrosion resistance is the
commonly
a MAO-treated coated
layer. with MAO
In addition, are Al, Mg, Ti, and their alloys [32]. High corrosion resistance is the
most important characteristic of abeing a porouslayer.
MAO-treated structure, this coating
In addition, being alayer
porousprovides high
structure, thisbone
most
ingrowth important
while characteristic of a MAO-treated layer. In addition, being a porous structure, this
coating layerformed
provides onhigh
biomedical implants
bone ingrowth whileand fixations
formed [33].
on biomedical implants and fixations [33].
coating layer provides high bone ingrowth while formed on biomedical implants and fixations [33].
Figure
Figure 3. 3. Schematicview
Schematic view of
of micro-arc
micro-arc oxidation
oxidation(MAO)
(MAO)process.
process.
Figure 3. Schematic view of micro-arc oxidation (MAO) process.
Advantages
Advantages of MAO
of MAO cancanbe abecoating
a coating surface
surface with with
highhigh hardness
hardness andand adherence
adherence propertieswhile
properties
Advantages of MAO can be a coating surface with high hardness and adherence properties
while
it haswhile it
differenthas different scales of porosity throughout its structure. This type of multi-structural nature
it hasscales of porosity
different throughout
scales of porosity its structure.
throughout This type
its structure. of multi-structural
This type of multi-structuralnature comes
nature
comes
fromcomes from
the coating the coating
itself. itself.
Figure 4 Figure
illustrates4 illustrates
a a MAO-treated
MAO-treated surface surface
under under different
different frequencies
frequencies resulting
from the coating itself. Figure 4 illustrates a MAO-treated surface under different frequencies
resulting in porous structures with different porosities. At the first steps of coating, a solid layer of
in porous structures
resulting with
in porous differentwith
structures porosities.
differentAtporosities.
the first steps
At theoffirst
coating,
stepsaofsolid layera of
coating, metallic
solid oxides
layer of
metallic oxides covers the substrate called barrier inner layer. The porous structure is created on top
covers the substrate
metallic calledthe
oxides covers barrier innercalled
substrate layer.barrier
The porous structure
inner layer. is created
The porous on topisofcreated
structure this layer during
on top
of this layer during the next steps of coating with a reported thickness of up to 100 μm [34]. This
of this
the next layer
steps ofduring
coatingthe nexta steps
with reportedof coating withof
thickness a reported
up to 100thickness
µm [34].ofThis 100 μmstructure
up toporous [34]. Thisis the
porous structure is the reason for increased surface adhesion in bio applications. The parameters
reasonporous structure
for increased is the
surface reason
adhesion for increased surface
in bio applications. adhesion in bio
Theelectrolyte
parameters applications.
affecting The parameters
affecting the coating quality are voltage, current density, type, processthe coating
time, quality
pulsate
affectingcurrent
are voltage, the coating quality are voltage, current density, electrolyte type,andprocess time,type,
pulsate
current, and current type, i.e., AC or DC [35,36]. However, many researchers utilized different AC
density, electrolyte type, process time, pulsate current, current i.e.,
current, and current type, i.e., AC or DC [35,36]. However, many researchers utilized different
or DC [35,36].
process However,
parameter many
ranges andresearchers
it has beenutilized
claimed different
that in allprocess parameter
the studies, corrosion ranges and itofhas
properties thebeen
process parameter ranges and it has been claimed that in all the studies, corrosion properties of the
claimed thatsamples
coated in all the studies, corrosion
improved while metallic properties of the decreased
ion release coated samples improved
significantly whileThe
[37–39]. metallic
only ion
coated samples improved while metallic ion release decreased significantly [37–39]. The only
disadvantage
release of the MAO process
decreased significantly [37–39].might be itsdisadvantage
The only limitation in substrate
of the MAO materials
processthatmight
are mostly
be its valve
limitation
disadvantage of the MAO process might be its limitation in substrate materials that are mostly valve
metals
in substrate such as Al,
materials Mg, Ti,
that Ti, Zr,
areZr, Nb,
mostly and Ta
valve [35].
metals such as Al, Mg, Ti, Zr, Nb, and Ta [35].
metals such as Al, Mg, Nb, and Ta [35].
Figure 4. SEM micrographs of MAO coating structures under different frequencies of (a) 60 Hz, (b)
FigureSEM
Figure 4. SEM micrographs
micrographs ofMAO
MAOcoating
of2000 coating structures
structures under
underdifferent
differentfrequencies of (a)
frequencies of60
(a)Hz,
60 (b)
Hz, (b)
5004.Hz, (c) 1000 Hz, and (d) Hz [40].
500 Hz, (c) 1000 Hz, and (d) 2000 Hz
500 Hz, (c) 1000 Hz, and (d) 2000 Hz [40].[40].
J.J. Manuf.
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Mater. Process.
Process. 2019,
2019, 3,
3, 28
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2.4. Electrodeposition Coating

2.4. Electrodeposition Coating
Electrodeposition of materials is considered a type of protection utilizing the deposition of
metallic ions on a substrate.
Electrodeposition In this is
of materials process,
considereda difference
a type ofinprotection
potential utilizing
between the anode and cathode
deposition poles
of metallic
causes
ions onan ion transfer
a substrate. in the
In this unit cell.
process, After a while,
a difference a coating
in potential layer forms
between anodeon and the submerged
cathode polessample
causes
by ion
an receiving
transferions in the from
unit thecell.other
After electrode.
a while, a Extensive
coating layer studies
formshave on the been done on
submerged popular
sample by
electrodeposition
receiving ions frommaterials. The common
the other electrode. Extensivegroup of metals
studies have been thatdone
have on been
popular intensively studied
electrodeposition
includes, but
materials. Theiscommon
not limitedgroup to,of
Ni-P,
metalsNi-P/Sn,
that haveNi-P-W,
been Ag/Pd, Cu/Ag,
intensively Cu/Ni,
studied Co/Ag,
includes, and
but Co/Pt
is not [41–
limited
43].Ni-P,
to, According
Ni-P/Sn, to Ni-P-W,
these studies,
Ag/Pd, theCu/Ag,
electrodeposited
Cu/Ni, Co/Ag, coatings
andsignificantly
Co/Pt [41–43]. enhance the corrosion
According to these
properties
studies, theofelectrodeposited
the substrate. Moreover, this technique
coatings significantly has been
enhance the shown
corrosion to be promising
properties in producing
of the substrate.
superhydrophobic
Moreover, polymeric
this technique has beencoatings
shown such
to beaspromising
polythiophene [44]. In superhydrophobic
in producing general, electrodeposition polymeric is
categorized
coatings such into
as two processes known
polythiophene [44]. In asgeneral,
electrolytic deposition (ELD)
electrodeposition and electrophoretic
is categorized into twodeposition
processes
(EPD), which
known are discussed
as electrolytic more (ELD)
deposition in the following sections. deposition (EPD), which are discussed
and electrophoretic
more in the following sections.
2.4.1. Electrolytic Deposition (ELD) Coating
2.4.1. Electrolytic Deposition (ELD) Coating
ELD is an electrochemical process employed to form a dense metallic coating with a uniform
thickness is
ELD an electrochemical
distribution on conductiveprocess employedSubstrate
substrates. to form aand dense metallicmaterials
deposition coating with a uniform
are selected as
thickness
cathode and distribution
anode while on conductive
placed inside substrates. Substrate and
an electrochemical unitdeposition
cell. Figure materials are selected
5 illustrates a generalas
cathode
overviewand of anode while placed
the process. inside aanpotential
By applying electrochemical
differenceunitbetween
cell. Figure
anode 5 illustrates
and cathode a general
poles,
overview of the process. By applying a potential difference between
metallic ions move toward working electrolyte and from there toward the substrate. The deposition anode and cathode poles,
metallic ions move
phase requires toward working
super-saturation electrolytewhich
of electrolyte, and from there
occurs due toward the substrate.
to charging current in Thethedeposition
circuit. In
phase requires super-saturation of electrolyte, which occurs due to charging
this technique, the concentration of metallic ions of electrolyte remains constant during the coating current in the circuit.
In this technique,
process [45]. Althoughthe concentration
this method of metallic ions ofused
is mostly electrolyte remains constant
for decorative during the coating
and low-corrosion/wear
process [45]. Although
applications, there have this
beenmethod
reports is mostly used for decorative
of development and low-corrosion/wear
of other applications such as optics,applications,
electronics,
there have been reports of development of other applications such as optics,
biomedical, high-temperature, and solid-oxide fuel cells [46,47]. By further increasing the potential electronics, biomedical,
high-temperature,
difference in electrolytic and solid-oxide fuel cellsmaterials
unit cells, ceramic [46,47]. can
By further increasing
be deposited the potential
on metallic difference
substrates that is
in electrolytic unit cells, ceramic materials can be deposited on metallic
more similar to the MAO process. Tian et al. [48] deposited Ni-Co-Al2O3 on steel pipes and reported substrates that is more
similar to the MAO process. Tian et al. [48] deposited
a notable enhancement of corrosion of substrate exposed to oil sand2 slurry. Ni-Co-Al O 3 on steel pipes and reported
Yang et al. [49] deposited
aNi-Co-SiC
notable enhancement
on carbon steel of corrosion of substrate
pipes exposed to oil exposed
sand slurryto oil
andsand slurry. significant
reported Yang et al. [49] deposited
corrosion and
Ni-Co-SiC on carbon steel pipes exposed to oil sand slurry and reported
erosion-enhanced corrosion resistance. The same results were reported by Fayomi et al. [50] on a Zn- significant corrosion and
erosion-enhanced
Ni-Al2O3-coated mild corrosion resistance.
steel substrate. The same
In addition, results were
Redondo reported
et al. [51] by Fayomi
deposited et al.resistant
a corrosion [50] on
apolypyrrole
Zn-Ni-Al2 O 3 -coated
(PPy) coatingmildonsteel substrate.
a copper substrateIn addition, Redondo et
from a dihydrogen al. [51] deposited
phosphate solution. a corrosion
resistant polypyrrole (PPy) coating on a copper substrate from a dihydrogen phosphate solution.
Figure 5. Schematic setup for electrodeposition of copper metal particles

particles over
over aluminum
aluminum oxide
oxide [52].
[52].
2.4.2.
2.4.2. Electrophoretic
Electrophoretic Deposition
Deposition (EPD)
(EPD) Coating
Coating
EPD
EPD isis another
another form
form ofof electrodeposition
electrodeposition that
that provides
provides thicker
thicker coating
coating layers
layers with
with aa colloidal
colloidal
nature. Using an
nature. Using an electric
electric field
field in
in a
a unit
unit cell,
cell, similar
similar to
to that
that of
of ELD,
ELD, thin
thin films
films form
form on
on substrates
substrates byby
coagulation of colloidal particles. EPD is a multi-phase technique, in
coagulation of colloidal particles. EPD is a multi-phase technique, in which:which:
J.J. Manuf.
Manuf. Mater.
Mater. Process. 2019, 3,
Process. 2019, 3, 28
x FOR PEER REVIEW 77 of
of 22
21
1. External electric field forces suspended particles in electrolyte toward one electrode called
1. External electric field forces suspended particles in electrolyte toward one electrode
electrophoresis.
called electrophoresis.
2. The moving particles gather in one electrode and form a larger coagulated particle.
2. The moving particles gather in one electrode and form a larger coagulated particle.
3. The larger particles deposit on the surface of the electrode, which is a to-be-coated substrate.
3. The larger particles deposit on the surface of the electrode, which is a to-be-coated substrate.
Finally, a thick coating layer will be created on the substrate having a powder-shaped structure.
Figure Finally, a thick coating
6 represents layer will
a schematic of be
thecreated
working on the substrateof
mechanism having
the EPD a powder-shaped structure.
process. Densification
Figure 6 represents a schematic of the working mechanism of the EPD process.
processes (e.g., furnace curing, light curing, sintering, etc.,) are recommended to increase the qualityDensification processes
(e.g.,
of thefurnace
protective curing,
layer.light
Up tocuring, sintering, applications
now, numerous etc.,) are recommended to increase
have been introduced forthe
EPD quality of the
that include
protective layer. Up to now, numerous applications have been introduced
coating, selective deposition, graded material deposition, porous structure deposition, and for EPD that include
coating,
biomedical selective deposition,
applications graded
[53,54]. Thematerial
materialsdeposition,
used in EPDporous structure deposition,
are commonly and biomedical
borides, carbides, oxides,
applications [53,54]. The materials used in EPD are commonly borides, carbides,
phosphates, and metals [53,55]. Castro et al. [56] reported fabricating corrosion resistant coatings by oxides, phosphates,
and metals
sol–gel and[53,55].
EPD onCastro et al. [56]AISI
stainless-steel reported
304 andfabricating
reportedcorrosion
two and fourresistant
times coatings
increasesby in
sol–gel and
corrosion
EPD on stainless-steel
resistance AISI 304
for each of these and reported
processes, two andInfour
respectively. timesstudy
another increases in corrosion
by Gebhart et al.resistance for
[57], an AISI
each of these processes, respectively. In another study by Gebhart et al. [57],
316 L stainless steel was coated with chitosan for biomedical applications. They reported positive an AISI 316 L stainless
steel
effectswasof coated with chitosan
this coating on corrosion for biomedical
behavior ofapplications.
the substrate.TheyTheyreported positive
also asserted effects
that of this
the applied
coating
electric on fieldcorrosion
in EPDbehavior
is the key of the substrate.
factor They also
in controlling asserted
coating that thesuch
features, applied electric field in
as hydrophobicity,
EPD is the key factor in controlling coating features, such as hydrophobicity,
thickness, and structure. TC4 Ti-alloy orthopedic implants were coated by graphene by thickness, andChen
structure.
et al.
TC4 Ti-alloy orthopedic implants were coated by graphene by Chen et al. [58].
[58]. They reported that the graphene-coated artificial joint implants show a considerable increase They reported that the
in
graphene-coated artificial joint implants show a considerable increase
life span. They found that the reason any corrosion on substrates occurred was micro-cracks in in life span. They found that
the reason
coating any corrosion
surfaces. Fei et al. on[59]substrates
studied the occurred was micro-cracks
wear resistance in coating
of EPD coatings and surfaces.
successfully Feideposited
et al. [59]
studied the wear
SiC particles resistance offriction
on paper-based EPD coatings
materialsandandsuccessfully
achieved deposited
an excellent SiCwear
particles on paper-based
enhancement of this
friction materials and achieved an excellent wear enhancement of
material. Table 1 summarizes ELD and EPD processes regarding their characteristics and this material. Table 1 summarizes
ELD and EPD processes regarding their characteristics and components.
components.
Figure 6. Sketch of the electrophoretic deposition process

process [60].
[60].
Table 1. Characteristics of electrodeposition techniques [61].

Table 1. Characteristics of electrodeposition techniques [61].
PropertyProperty ELD ELD EPD EPD
CoatingCoating
elementselements Ions Ions Solid particles
Solid particles
Surface Surface
charge charge Medium
Medium High High
Preferred electrolyte Water Organic
Preferred electrolyte
Ionic electrolytic strength High
Water OrganicLow
Ionicconductivity
Electrolytic electrolytic strength HighHigh Low Low
ApproximateElectrolytic conductivity 0.1 µm/min
rate of deposition High Low
1000 µm/min
Approximate rate of deposition 0.1 μm⁄min 1000 μm⁄min
J. Manuf.
2.5. Mater.
Sol–gel Process. 2019, 3, 28
Coating 8 of 22
Sol–gel coating is one of the most successful coating processes of biomedical devices. The wide
2.5.
rangeSol–gel Coating
of investigations on this process and its applications can ease the setup and performance of
experiments while keeping
Sol–gel coating is one of the
the outcomes reliable
most successful [62]. processes
coating On the other hand, sol–gel
of biomedical is capable
devices. The wide of
enhancing previously existing coating layers from corrosion and ion release
range of investigations on this process and its applications can ease the setup and performance point of view. Due to its
liquid-permeating
of experiments while nature, sol–gel
keeping can easilyreliable
the outcomes seal porous coating
[62]. On structures
the other or damaged
hand, sol–gel layers.
is capable of
Calcium phosphorous
enhancing (CaP) precursors
previously existing coating layersdissolved in ethanol/distilled
from corrosion water
and ion release are of
point used
view. to Due
maketothe its
solution called asnature,
liquid-permeating Sol. Insol–gel
order canto make a gel
easily seal phasecoating
porous out ofstructures
the solution, the prepared
or damaged mixture
layers. Calcium
undergoes heating
phosphorous (CaP) at different dissolved
precursors temperatures to facilitate the aqueous
in ethanol/distilled water areportion
used toofmake
the solution and
the solution
increase the viscosity to the desired level. This phase, which transforms it from a liquid
called as Sol. In order to make a gel phase out of the solution, the prepared mixture undergoes heating solution to a
gel phase, is where sol–gel gets its name. After preparation, the parts or devices
at different temperatures to facilitate the aqueous portion of the solution and increase the viscosity are dipped in the
sol–gel
to medium
the desired at aThis
level. constant
phase,andwhichcontrolled
transformsspeed. Thisa process
it from may betorepeated
liquid solution to achieve
a gel phase, is wherea
multilayered coating or thicker coating of the same material. In addition, the
sol–gel gets its name. After preparation, the parts or devices are dipped in the sol–gel medium coated samples canatbe a
baked to dry out faster or to provide intentional dehydrating cracks on the
constant and controlled speed. This process may be repeated to achieve a multilayered coating or surface of the coating
layer for
thicker next processing
coating of the samesteps. Figure
material. 7 represents
In addition, a schematic
the coated samples of an
canexample
be bakedoftoadrysol–gel coating
out faster or
process.
to provide intentional dehydrating cracks on the surface of the coating layer for next processing steps.
Figure 7 represents a schematic of an example of a sol–gel coating process.
Figure 7. Schematic
7. Schematic sol–gel
sol–gel coating
coating process
process from solution
from solution preparation
preparation to the
to the final final
solid solid
structure
structure
formation.formation.
Advantages
Advantages of of the
the sol–gel
sol–gel process
process include
include high
high adhesion
adhesion of of the
the coating
coating layer,
layer, ability
ability toto coat
coat
complex geometries, flexibility in the composition of the coating layer,
complex geometries, flexibility in the composition of the coating layer, and lower cost than other and lower cost than other
similar
similar coating
coating processes. Additionally, there
processes. Additionally, there isis no
no need
need to to have
have aa conductive
conductive material
material as as aa substrate
substrate
as
as there
there is
is no
no extreme
extreme heating
heating oror vacuum
vacuum applied
applied to to the
the parts
parts meaning
meaning that that the
the substrate
substrate will
will bebe
virtually untouched during the coating process. Sol–gel coating is done
virtually untouched during the coating process. Sol–gel coating is done in different forms such as in different forms such
as dip-coating,
dip-coating, spraying,
spraying, andand spinning
spinning [63,64].
[63,64]. FigureFigure
8 shows 8 shows a sol–gel
a sol–gel deposited
deposited coatingcoating
layer withlayera
with
rougha and
rough and porous
porous microstructure.
microstructure. One disadvantage
One disadvantage of this could
of this process process becould
that abe that a constant
constant speed of
speed of dipping and withdrawing is needed to maintain a uniform
dipping and withdrawing is needed to maintain a uniform thickness of coating throughout the thickness of coating throughout
the substrate
substrate surface.
surface. There There is also
is also alwaysalways a possibility
a possibility of coating
of coating failure
failure during
during heatheat treatment
treatment on
on multilayered coating structures. Sol–gel coating for industrial applications
multilayered coating structures. Sol–gel coating for industrial applications is considered a slow is considered a slow
process
process and
and isis not
not cost
cost effective
effective in
in high
high production
production rates
rates [65].
[65]. All
All these
these being said, the
being said, the sol–gel
sol–gel process
process
performs
performs well
well when
when it it comes
comes to to protecting
protecting aa substrate
substrate against corrosion and
against corrosion and decreasing
decreasing ion ion release,
release,
as reported in many scientific studies [66,67]. Moreover, in a study by Faustini,
as reported in many scientific studies [66,67]. Moreover, in a study by Faustini, et al. [68], models et al. [68], models were
proposed in order to explain and predict sol–gel behavior
were proposed in order to explain and predict sol–gel behavior and the effect ofand the effect of dipping/withdrawing
steps on the final quality
dipping/withdrawing of the
steps oncoating
the final layer. Likewise,
quality of themanycoatingother studies
layer. investigated
Likewise, many andother proposed
studies
continuum-based/numerical models that could be implemented
investigated and proposed continuum-based/numerical models that could be implemented in in predicting sol–gel mechanisms
during the sol–gel
predicting processmechanisms
and characteristics
duringofthe theprocess
coatingand layers [69–73]. Hybrid
characteristics of thenetwork
coating materials were
layers [69–73].
generated using sol–gel
Hybrid network materials process
were when
generated either organic
using moieties
sol–gel process or polymeric
when either categories chemically
organic moieties or
bonded to an inorganic component. The chemical bond between the
polymeric categories chemically bonded to an inorganic component. The chemical bond between organic and inorganic networkthe
J. Manuf. Mater. Process. 2019, 3, 28
x FOR PEER REVIEW 99 of
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22
organic and inorganic network can be addressed through introducing functional groups into the
can be addressed
polymeric part bythrough introducing
silane, silanol, functional
etc., using groups into
pre-introduced the polymeric
functional groupspart by silane,
in the silanol,
polymer, and
etc., using pre-introduced functional groups in the polymer, and exploiting alkoxysilanes
exploiting alkoxysilanes precursors. Poly(dimethylsiloxane) (PDMS), poly(ether ketone) (PEK) , and precursors.
Poly(dimethylsiloxane)
polycarbonate are among (PDMS),
numerouspoly(ether
polymericketone) (PEK),that
materials andhave
polycarbonate
been used inarethe
among numerous
sol–gel process
polymeric
[74–77]. materials that have been used in the sol–gel process [74–77].
8. SEM
Figure 8. SEM of
ofsol–gel-deposited
sol–gel-depositedCaP
CaPmicrostructure
microstructure in different
in different magnifications
magnifications of same
of the the same area
area [78].
[78].
2.6. Thermal Spray Coating
2.6. Thermal
ThermalSpray
sprayCoating
coating is a general term for a series of processes that utilize a plasma, electric,
or chemical
Thermalcombustion
spray coating heatis asource
generaltoterm
meltfora set of designed
a series materials
of processes and spray
that utilize the melt
a plasma, on the
electric, or
surface in order to produce a protective layer. These are reliable types of corrosion-
chemical combustion heat source to melt a set of designed materials and spray the melt on the surface and wear-resistant
coatings.
in order to In this process,
produce a heat source,
a protective layer.which
Theseis mostly provided
are reliable typesbyofchemical
corrosion-combustion or plasma
and wear-resistant
discharge,
coatings. Inheats up the materials
this process, to a molten
a heat source, which isormostly
semi-solid phaseby
provided and sprays combustion
chemical them on theor substrate
plasma
with a high speed of a jet. The thickness achieved in thermal spray coating
discharge, heats up the materials to a molten or semi-solid phase and sprays them on the substratetechniques can range from
20 µm to several millimeters which is significantly higher than the thickness offered
with a high speed of a jet. The thickness achieved in thermal spray coating techniques can range from by electroplating,
CVD,
20 μmortoPVD processes
several [79]. In which
millimeters addition, is the materials that
significantly can than
higher be used theasthickness
feedstock offered
of thermal by
spray coatings range from refractory metals and metallic alloys to ceramics,
electroplating, CVD, or PVD processes [79]. In addition, the materials that can be used as feedstockplastics, and composites
and can easily
of thermal spraycover a relatively
coatings range from highrefractory
surface area of aand
metals substrate
metallic [79]. Thermal
alloys spray plastics,
to ceramics, coatingsand
are
categorized
composites and into can
different
easilytypescoverbased on theirhigh
a relatively characteristics
surface area andof process specifications.
a substrate Thespray
[79]. Thermal most
popular categories are plasma, detonation, warm/cold, high-velocity air fuel (HVAF),
coatings are categorized into different types based on their characteristics and process specifications. high-velocity
oxyfuel
The most (HVOF),
popularflame, and wire
categories arc spraying
are plasma, [80,81].warm/cold, high-velocity air fuel (HVAF), high-
detonation,
velocity oxyfuel (HVOF), flame, and wire arc spraying [80,81].
2.6.1. High-Velocity Oxy-Fuel Coating (HVOF)
2.6.1.Figure
High-Velocity Oxy-Fuel
9a represents Coating
an HVOF (HVOF)
coating process in a schematic format. A mix of fuel, such as
acetylene, propane, methane, hydrogen, or natural gas, and oxygen in gas or liquid phase undergo
Figure 9a represents an HVOF coating process in a schematic format. A mix of fuel, such as
continuous combustion in a designed combustion chamber to provide a high-pressure steam of hot
acetylene, propane, methane, hydrogen, or natural gas, and oxygen in gas or liquid phase undergo
gas. The combustion chamber releases the combustion products into a nozzle to create a spray with a
continuous combustion in a designed combustion chamber to provide a high-pressure steam of hot
speed of more than 1000 m/s [82]. After combustion, coating materials in powder form are injected
gas. The combustion chamber releases the combustion products into a nozzle to create a spray with
inside this hot jet stream to get partially melted accelerated while they are leaving the nozzle tip.
a speed of more than 1000 m/s [82]. After combustion, coating materials in powder form are injected
The hot jet pushes the semisolid particles against the substrate and creates a coating layer with varying
inside this hot jet stream to get partially melted accelerated while they are leaving the nozzle tip. The
thicknesses up to several millimeters. The advantage of this process is that the coating layer has a
hot jet pushes the semisolid particles against the substrate and creates a coating layer with varying
high density and adheres to the substrate well, while it is able to utilize coating materials such as
thicknesses up to several millimeters. The advantage of this process is that the coating layer has a
hydroxyapatite (HA), W, Cr, Al, Zr, and their oxides/carbides or polymeric materials such as nylon
high density and adheres to the substrate well, while it is able to utilize coating materials such as
11/silica nanocomposites to deposit corrosion- and wear-resistant layers [83,84]. Figure 9b represents
hydroxyapatite (HA), W, Cr, Al, Zr, and their oxides/carbides or polymeric materials such as nylon
a multilayer coating provided by HVOF. The coating layer could be performed on non-conductive
11/silica nanocomposites to deposit corrosion- and wear-resistant layers [83,84]. Figure 9b represents
materials such as polymers and ceramics that are able to undergo high velocity and temperature of
a multilayer coating provided by HVOF. The coating layer could be performed on non-conductive
the jet stream and the particle [85]. To date, many researchers have investigated corrosion and wear
materials such as polymers and ceramics that are able to undergo high velocity and temperature of
resistance of HVOF coatings in various applications and corrosive environments. Based on these
the jet stream and the particle [85]. To date, many researchers have investigated corrosion and wear
studies, coating layers made by this technique served well and improved corrosion-wear properties of
resistance of HVOF coatings in various applications and corrosive environments. Based on these
substrates [86–88]. A summary of these studies is listed in Table 2.
studies, coating layers made by this technique served well and improved corrosion-wear properties
of substrates [86–88]. A summary of these studies is listed in Table 2.
(a) (b)
Figure 9.9.(a)(a)
Figure Schematic
Schematic setup
setup of aofhigh-velocity
a high-velocity oxy-fuel
oxy-fuel (HVOF)
(HVOF) coating
coating systemsystem [89]
[89] and (b)and (b)
cross-
cross-section
section SEM micrograph
SEM micrograph of HVOF-sprayed
of HVOF-sprayed multilayer
multilayer coating
coating on Al7075-T7351
on Al7075-T7351 platesplates
[87]. [87].
Table 2. Electrochemical corrosion measurements of different coating composition provided by

Table 2. Electrochemical corrosion measurements of different coating composition provided by
HVOF [90].
HVOF [90].
Coating Composition Corrosion Rate (mm/y)
Coating Composition
0.1M NaOH
Corrosion Rate (mm/y)
0.1M H2 SO4 Sea Water
0.1M NaOH 0.1M H2SO4 Sea water
WC−Cr3 C2 −Ni 0.38 0.15 −
WC−Cr3C2−Ni 0.17
Cr3 C2 −NiCr 0.38 0.15
0.077 − −
WC−Co Cr3C2−NiCr − 0.17 0.077
− − 0.76
WC−Co−Cr WC−Co − − −− 0.76 0.32
Cr2 O3 −Al2 O3 −WC−Co−Cr
TiO2 3.2 ×10−5 − 3.6 ×−10−5 0.32 −
Cr2 O3 7.6 ×10−3 1.5 ×10−3 −
Cr2O3−Al2O3−TiO2 3.2 × 10 3.6 × 10 −
Cr2O3 7.6 × 10 1.5 × 10 −
2.6.2. Plasma Spray Coating
2.6.2.Figure
Plasma10Spray Coating
illustrates a schematic view of a plasma spray coating setup. This process can be done
under vacuum or atmospheric
Figure 10 illustrates a schematic conditions.
view of In athis process,
plasma a plasma
spray coatinggun provides
setup. a high-temperature
This process can be done
DC/induction plasma (up to 10000 K), which can easily melt refractory metals,
under vacuum or atmospheric conditions. In this process, a plasma gun provides a high-temperature ceramics, and polymers.
The materials used in the stabilization of plasma can be gas, water,
DC/induction plasma (up to 10000 K), which can easily melt refractory metals, ceramics, or a mixture of these two, known
and
as hybrid The
polymers. plasma. The materials
materials used in the to stabilization
be depositedofare fed into
plasma canthis hot plasma
be gas, water, or stream and the
a mixture high
of these
temperature
two, known as melts the feedstock.
hybrid plasma. The Due to the high
materials to be speed of plasma
deposited at the
are fed tipthis
into of ahot
converging nozzle,and
plasma stream the
molten droplets are deposited instantly on the substrate against the coating setup.
the high temperature melts the feedstock. Due to the high speed of plasma at the tip of a converging The flexibility of this
processthe
nozzle, facilitates
moltenthe utilization
droplets of different
are deposited types ofon
instantly feedstock such as
the substrate powder,
against the slurry,
coatingsuspensions,
setup. The
and liquids [91]. The resulting coating layer has a high corrosion and wear resistance
flexibility of this process facilitates the utilization of different types of feedstock such as powder, and it is able
to adhere to the substrate due to surface tension and high temperature. A
slurry, suspensions, and liquids [91]. The resulting coating layer has a high corrosion and wear significant corrosion- and
wear-resistance
resistance and itenhancement
is able to adherewas reported in manydue
to the substrate studies on different
to surface tensionmaterials
and high such as chromium
temperature. A
significant corrosion- and wear-resistance enhancement was reported in many studies onhave
oxide and NiCr alloys [92,93]. Plasma sprayed coating of polymers, especially PEEK, been
different
implemented
materials suchforascorrosion
chromium protection
oxide and of metal substrates
NiCr alloys (nylon,
[92,93]. PVDF),
Plasma antistick
sprayed coatings
coating of papers
of polymers,
especially PEEK, have been implemented for corrosion protection of metal substrates (nylon,electrical
and rollers, plastic moldings, wear-resistant coatings, moisture protection materials, and PVDF),
barrier coatings
antistick coatings[94]. On theand
of papers other hand,plastic
rollers, vacuum plasma wear-resistant
moldings, spraying is a low-temperature
coatings, moisture process and is
protection
mostly used
materials, andforelectrical
materialsbarrier
that cannot perform
coatings [94]. Onreactions in atmospheric
the other hand, vacuum pressure
plasma to modify
spraying the
is surface
a low-
of the substrate. The most popular application of vacuum plasma spraying
temperature process and is mostly used for materials that cannot perform reactions in atmospheric is the surface modification
of engineering
pressure polymers
to modify and plastics,
the surface of the rubbers,
substrate. metals, and fibers
The most popular[95]. In this process,
application a material
of vacuum plasmacan
go through
spraying cross-linking,
is the friction decrease,
surface modification adherence
of engineering increase,
polymers etc.
and [95–97].
plastics, rubbers, metals, and fibers
[95]. In this process, a material can go through cross-linking, friction decrease, adherence increase,
etc. [95–97].
Figure 10. Schematic [98]..

Schematic plasma spray coating setup and its parts [98]
Figure 10. Schematic plasma spray coating setup and its parts [98].
2.6.3. Cold
2.6.3. Cold Spray
Spray Coating
Coating
2.6.3. Cold Spray Coating
Cold spray
Cold spray coating
coating is is a
a technique
technique thatthat relies
relies on
on impact
impact and and solid
solid mechanics
mechanics of of particles. Unlike
particles. Unlike
HVOF Cold
and spray
plasma coating
spray is a technique
coating methods, thatthis
relies on impact
process does and
not solidamechanics
utilize heat source oftoparticles.
perform Unlike
coating
HVOF and plasma spray coating methods, this process does not utilize a heat source to perform
HVOF and
on substrates. plasma spray
The general coating methods,
workingworking
mechanism this process does
of cold spray not
coatingutilize a heat source to perform
coating on substrates. The general mechanism of cold spray depends on particle
coating depends on size, the
particle
coating
temperatureon substrates.
of the target, The general working mechanism of cold spray coating depends on particle
size, the temperature of thematerial properties
target, material of coating
properties ofparticles, and a critical
coating particles, and avelocity [99]. Powder
critical velocity [99].
size, the temperature
materials are fed to a of the target,
stream of material properties
high-velocity mediums of(helium
coatingandparticles, and to
nitrogen) a critical
achieve velocity [99].
the desired
Powder materials are fed to a stream of high-velocity mediums (helium and nitrogen) to achieve the
Powderenergy.
kinetic materials areparticle-substrate
fed to a stream ofimpacts high-velocity mediums (helium and nitrogen) to achieve the
desired kinetic After
energy. After particle-substrate take place,
impacts thisplace,
take energy deforms
this energythe particles
deforms theand bond
particles
desired
thembond kinetic
to the energy.
substrate. After particle-substrate
Another mechanism impacts
of this process take
can place, this
be penetrationenergy deforms
of the particles the particles
and them to the substrate. Another mechanism of this process can be penetration of theinside the
particles
and bond them
substrate. Using toathe
high substrate.
flow rateAnother
of mechanism
accelerated of this
particles, process
the surface can
is be penetration
coated with of thematerials.
desired particles
inside the substrate. Using a high flow rate of accelerated particles, the surface is coated with desired
inside
The the substrate.
most-used powder Using a high flow rateofofaaccelerated
materials particles, the surface ceramics,
is coated with desired
materials. The most-used powderconsist wide range
materials consist of plastics,
of a wide range metals,
of plastics, metals, composites,
ceramics,
materials.
and metallicandThe most-used
alloys [100,101]. powder materials
In[100,101].
addition, In consist
theaddition, of
most-studied a wide range of plastics,
substrate materials metals, ceramics,
composites, metallic alloys the most-studied substrateinclude softinclude
materials metals
composites, andCu, metallic alloys [100,101]. In addition, the hard
most-studied substrate materials include
soft metals such as Al and Cu, while in literature, the coating of some hard materials such as Wbeen
such as Al and while in literature, the coating of some materials such as W and Ti has and
soft metals
reported such as In
[102,103]. Alsome
and Cu, whilethe
studies, intemperature
literature, the of coating of some medium
the accelerating hard materials
hasmediumsuch
been as W and
increased in
Ti has been reported [102,103]. In some studies, the temperature of the accelerating has been
Ti hasto
order been reported
enhance [102,103].
process In some
efficiency studies,
[104]. Although the temperature
this process ofsimple
is the accelerating
and cheap medium
compared hastobeen
the
increased in order to enhance process efficiency [104]. Although this process is simple and cheap
increased
other thermalin order
spray to enhancethe
methods, process efficiency
operation range [104].
veryAlthough this process is simple and cheap
compared to the other thermal spray methods, theisoperation
limited.
rangeFigure
is very11 limited.
shows SEM micrographs
Figure 11 shows
compared
of cold to the
spray-treated other thermal
surfaces spray
and a methods,
schematic the
view operation
of cold range
spray is
coatingvery limited.
process. Figure 11 shows
SEM micrographs of cold spray-treated surfaces and a schematic view of cold spray coating process.
SEM micrographs of cold spray-treated surfaces and a schematic view of cold spray coating process.
Figure 11. Top: SEM micrographs of cold spray-coated AA6061 substrate by (a) as-received and (b)
Figure 11. Top:
Top:SEM
SEMmicrographs
micrographsofofcold
coldspray-coated
spray-coatedAA6061
AA6061 substrate
substrateby by
(a) (a)
as-received andand
as-received (b)
heat-treated AA7075 particles with a mechanical interlocking between the coating and the substrate
heat-treated
(b) AA7075
heat-treated particles
AA7075 with awith
particles mechanical interlocking
a mechanical betweenbetween
interlocking the coating
the and the substrate
coating and the
[105]. Bottom figure: a schematic view of cold spray coating process [106].
[105]. Bottom
substrate figure:
[105]. a schematic
Bottom view of cold
figure: a schematic spray
view coating
of cold sprayprocess
coating[106] .
process [106].
2.6.4. Warm Spray Coating

Figure 12 (left) shows a schematic representation of the warm spray coating method. As stated
about cold spray coating, low working temperature decreases efficiency and reliability of thermal
about cold spray coating, low working temperature decreases efficiency and reliability of thermal
spray coating methods. However, high temperatures melt feedstock and introduce new chemical
spray coating methods. However, high temperatures melt feedstock and introduce new chemical
reactions, which may cause oxidation or change of properties due to extreme heating of particles and
reactions, which may cause oxidation or change of properties due to extreme heating of particles and
substrates. In order to overcome this problem, a new technique was introduced as a warm spray
substrates. In order to overcome this problem, a new technique was introduced as a warm spray
coating. This is a modification of HVOF coating that enjoys reduced temperature in the combustion
coating. This is a modification of HVOF coating that enjoys reduced temperature in the combustion
chamber by introducing nitrogen to the fluid mixture. As a result, this method is categorized
chamber by introducing nitrogen to the fluid mixture. As a result, this method is categorized

about cold spray coating, low working temperature decreases efficiency and reliability of thermal spray
coating methods. However, high temperatures melt feedstock and introduce new chemical reactions,
which may cause oxidation or change of properties due to extreme heating of particles and substrates.
In order to overcome this problem, a new technique was introduced as a warm spray coating. This is
a modification of HVOF coating that enjoys reduced temperature in the combustion chamber by
introducing nitrogen to the fluid mixture. As a result, this method is categorized somewhere between
cold spray coating and HVOF coating and provides a high efficiency of the coating process [107].
However, as reported in the literature, the achieved coating layer contains many impurities relative to
the other two processes due to low temperature and existence of oxygen in the accelerating stream.
These porosities and oxide phases are illustrated in Figure 12 (right). Advantages of using this
process rise in the coating of materials, which are sensitive to oxidization in high temperatures or
the materials that cannot withstand high working temperatures such as bio-metal-glasses, Ti and its
alloys, engineering plastics, and polymers such as PEEK [108,109]. Cold/warm spray coatings are
not used for extremely harsh environments, however many research studies investigated corrosion
properties of this type of coating on different materials such as Ti, bio-metal-glasses, WC-Co cermet,
etc., under different corrosion conditions and they claimed an enhancement in corrosion resistance of
substrates [110,111].
2.6.5. Arc Wire Spray Coating

Another type of thermal spray coating technique is called arc wire spray coating (Figure 13a).
In this process, two consumable metallic wires, which are charged with a DC supply, generate an
arc between them resulting in a melting process of the feeding wires. The products of this melting
process are then pumped out of a converging nozzle tip toward the target with the supplied pressure
of compressed gas. Although the flexibility of this process allows for the use of many metallic alloys as
coating layers, this process is limited to conductive wires and materials. In order to solve this issue,
a modified version of arc wire plasma was introduced having one consumable wire, which makes an
arc with a non-consumable metallic cathode [112]. The remaining steps of the process are the same
as the original version. This method is well-known for applications of an internal surface coating
such as engine blocks, etc., that offers a lighter metal as the whole block while the internal surfaces
are coated with a wear- and corrosion-resistant metallic alloy. This flexibility can significantly reduce
production cost. Almost all of the conductive materials such as Al, Zn, Mo, Ni, and other metallic
alloys such as Ni and Ti alloys can be used as feedstock in this process [79,113]. In addition, utilization
of cored wires is reported in the literature [114]. Figure 13b represents the microstructure of an arc
wire spray-coated substrate. To this point, many of the popular thermal spray coating techniques have
been introduced. However, there is no doubt that other processes could be investigated regarding their
working mechanisms, coating efficiency, coating quality, speed of process, and ease of applications.
production cost. Almost all of the conductive materials such as Al, Zn, Mo, Ni, and other metallic
alloys such as Ni and Ti alloys can be used as feedstock in this process [79,113]. In addition, utilization
of cored wires is reported in the literature [114]. Figure 13b represents the microstructure of an arc
wire spray-coated substrate. To this point, many of the popular thermal spray coating techniques
have been introduced. However, there is no doubt that other processes could be investigated
regarding their working mechanisms, coating efficiency, coating quality, speed of process, and ease
of applications.
Figure
J. Manuf. Mater.12. Left:2019,
Process. A schematic of warm
3, x FOR PEER spray coating technique and its setup [115]. Right: Cross-section
REVIEW 13 of 21
Figure 12. Left: A schematic of warm spray coating technique and its setup [115]. Right: Cross-section
BSE micrographs of warm spray-deposited Ti-6Al-4V on low-carbon steel substrate processes spray
BSE micrographs of warm spray-deposited Ti-6Al-4V on low-carbon steel substrate processes spray
1.5 m3/min,
pressure and(d) 4 MPa flow
nitrogen and 0.5 m3/min,
rates of (a) 1 (e)
MPa 4 MPa andm3/min,
and 0.5 1 m3/min,
(b) and (f) and
1 MPa 4 MPa and 1.5 (c)
1 m3/min, m3/min,
1 MPa
pressure and nitrogen flow rates of (a) 1 MPa and 0.5 m3/min, (b) 1 MPa and 1 m3/min, (c) 1 MPa and
respectively [116].(d) 4 MPa and 0.5 m3/min, (e) 4 MPa and 1 m3/min, and (f) 4 MPa and 1.5 m3/min,
and 1.5 m3/min,
respectively [116].
Figure13.
Figure (a)Schematic
13. (a) Schematicarc arcwire
wirespray
spraycoating
coatingsetup
setup and
and mechanism
mechanism ofof operation
operation [117].
[117]. (b)
(b)SEM
SEM
micrograph of
micrograph of arc
arcwire
wirespray-coated
spray-coated surface by Tafa’s
surface steel (95MXC)
by Tafa's cored wire
steel (95MXC) coredfeedstock. The substrate
wire feedstock. The
material is
substrate not mentioned
material in Reference
is not mentioned [114].
in Reference [114].
3. Summary
3. Summary
In order to have a successful coating deposition on a substrate, there are several affecting
In order to have a successful coating deposition on a substrate, there are several affecting
parameters including deposition materials, substrate materials, feedstock form (powder, wire, rods,
parameters including deposition materials, substrate materials, feedstock form (powder, wire, rods,
precursors, etc.), and deposition methods. However, the deposition processes are the most important
precursors, etc.), and deposition methods. However, the deposition processes are the most important
ones as they deal with chemical alteration of materials and alloying of composition elements in the
ones as they deal with chemical alteration of materials and alloying of composition elements in the
coating layer. In addition, based on the characteristics of different feedstock and substrate materials,
coating layer. In addition, based on the characteristics of different feedstock and substrate materials,
one can easily choose the best option for deposition. The processes that are the most successful and the
one can easily choose the best option for deposition. The processes that are the most successful and
most investigated deposition means are physical/chemical vapor deposition (PVD/CVD), micro-arc
the most investigated deposition means are physical/chemical vapor deposition (PVD/CVD), micro-
oxidation (MAO), electrodeposition (i.e., electrolytic deposition (ELD) and electrophoretic deposition
arc oxidation (MAO), electrodeposition (i.e., electrolytic deposition (ELD) and electrophoretic
(EPD)), sol–gel, and different types of thermal spraying processes (i.e., HVOF, plasma, cold, warm, and
deposition (EPD)), sol–gel, and different types of thermal spraying processes (i.e., HVOF, plasma,
arc wire spraying). The mentioned processes utilize different mechanisms in order to deposit specific
cold, warm, and arc wire spraying). The mentioned processes utilize different mechanisms in order
types of materials on substrates making the material selection important in order to have the highest
to deposit specific types of materials on substrates making the material selection important in order
efficiency of the coating. Some of the processes use thermal sources to change the state of feedstock
to have the highest efficiency of the coating. Some of the processes use thermal sources to change the
to liquids and semisolids in forms of particles, droplets, and clusters. Some others use the difference
state of feedstock to liquids and semisolids in forms of particles, droplets, and clusters. Some others
between electrochemical charges between poles and some deposit materials without chemical change
use the difference between electrochemical charges between poles and some deposit materials
of state. Depending on the substrate materials, feedstock, and means of deposition, the coating layers
without chemical change of state. Depending on the substrate materials, feedstock, and means of
deposition, the coating layers are different in thickness, microstructure, and functionality. In
addition, some processes are specific to metallic feedstocks, which are conductive, while the rest can
deposit polymers, ceramics, and metallic alloys regardless of their physical properties.
In summary, the thermal processes, such as various types of thermal spray coating, implement
high temperatures and high speed of plasma jets in order to have a higher material deposition rate.
are different in thickness, microstructure, and functionality. In addition, some processes are specific to
metallic feedstocks, which are conductive, while the rest can deposit polymers, ceramics, and metallic
alloys regardless of their physical properties.
In summary, the thermal processes, such as various types of thermal spray coating, implement
high temperatures and high speed of plasma jets in order to have a higher material deposition
rate. In these methods, the high temperatures and high-speed jets allow feedstock deposition and
eliminate the adverse effects of high melting point on ceramics and superalloys. The obtained
coating thicknesses, in these cases, are high (up to several hundred microns). However, the coating
microstructure consists of oxide and carbide inclusions and provides porosity, depending on process
parameters. In the vaporization-based processes, the deposited coating layer is a thin film with
high corrosion/wear-resistance mostly used in tool coating and protection of sliding components
of machines. The coating achieved in these types is a thin solid film with low porosity and high
adherence to the substrate. Micro-arc oxidation is a high-voltage version of anodization, which is
mostly implemented on biomaterials for bone implant and biomedical device applications. In addition,
valve metals (Al, Ti, Zr, Hf, V, Nb) have been extensively used as substrates as well. The coating
structured by MAO offers high substrate/coating adhesion with a porous structure that is crucial
for biomaterial coating as the bone ingrowth increases. The porous microstructure also enhances
the corrosion resistance and facilitates the engineering calculations on the lifetime of the implants,
either degrading fast or staying for a longer time. Sol–gel is another type of material deposition that is
significantly flexible in feedstock composition, and as the process utilizes aqueous solutions as particle
carriers, the complexity of geometry does not affect the coating quality. In addition, sol–gel-deposited
layers are a reliable sealant for porous substrates and coatings in order to increase their corrosion
resistance. Although sol–gel offers high flexibility and capability in coating purposes, the process
is relatively slow and increases the production time. Electrochemical processes are another type of
aqueous deposition methods utilizing the difference between electrochemical charges of anode and
cathode poles of a chemical unit cell. The flexibility in the coating composition and a wide variety of
substrates used in this method make it a reliable deposition process. However, this process suffers
from depending on conductivity properties of substrates (poles) for material deposition as the charges
need to move freely in the circuit.
Although these processes are reliable means of material deposition and surface protection, there
are disadvantages to all of them in different applications. Thus, there have been studies on combining
these techniques in order to benefit from an advantageous point of each process and minimize the
negative effect of each method. The most applicable way of deposition modification and protection
enhancement is known to be multilayered coating deposition. The different layers deposited on top
of the previous ones can have different thicknesses, compositions, and physical/chemical properties.
This consideration has more importance while porous structures or thin films are deposited. As an
instance, a PVD-coated substrate has a thin film with notable corrosion/wear resistance, but a higher
layer thickness can increase the functional lifetime of the coated component. As another example,
the porous microstructure of a MAO-treated surface can be sealed with several layers of sol–gel
deposition in order to decrease the corrosive medium penetration to the substrate and increase its
corrosion resistance while maintaining the porous structure. All being said, in order to have the highest
efficiency and functionality of a protective layer, different aspects need to be considered carefully.
Layer thickness, coating composition, suitability of the deposition technique regarding feedstock and
substrate materials, and physical/chemical properties of the deposited layers are the key features
changing the final protection quality. Table 3 presents a brief overview of the discussed processes and
their features. In addition, pros and cons of covered coating techniques in this review are summarized
in Table 4.
Table 3. Summary of coating processes and their specific feature.
Deposition Process Source Feedstock Material Substrate Material Coating Thickness (µm) Reference
AISI M2 steel, SS, glass, Si,
TiCxOy-ZrCxOy, TiN, PE, PVDF, potassium
PVD Physical 1.2–6.3, 5, 0.2, 0.2, 0.1, 0.1 [10,11,17,18,118]
PTh bromide(KBr)-carbon-Au-Al,
Ag-Au-Cu-Al
Niobium oxide(Nb2 O5 ),
W-TiN-WSi2 -Ta2 O5 -Cu-SiO2 , 0.05–0.2, -, 0.2–0.6,
CVD Chemical Glass, Si, Si, Kleenex, Ni-Co-Fe [24,25,119–121]
polycrystalline Si- Si3 N4 -SiO2 , 0.04–0.1–16
PTFE, Ni3 Ti
Hydroxyapatite (HA)/TiO2 , PCL
MAO Electrochemical Ti-6Al-4V, Mg, NiT 10–20, 2–3, 7 [32,34,37]
duplex, HA- HA/ZrO2
Ni-Co-Al2 O3 , Ni-Co-SiC,
ELD Electrochemical Steel, carbon steel, mild steel, Cu 50–200, 10–70, -, - [48–51]
Zn-Ni-Al2 O3 , PPy
AISI 316L SS, AISI 304 SS, AISI
bioactive glass (45S5
316 L SS, Ti-6Al-4V alloy (TC4),
EPD Electrochemical BG)-Cu-doped BG, SiO2 , -, 7, 1–6, -, - [56–59,122]
Aramid-carbon-cellulose fibers
chitosan, grapheme, SiC
composite
TiCl4 -(tetraethyl orthosilicate)
TEOS- (methyltriethyl
Sol–gel Physical Si, NiTi, stainless steel 0.01–1, 1–4 [62,68,74,123],
orthosilicate)MTEOS, HA, PDMS,
Polycarbonate
Ti-6Al-4V, Inconel 738 metal, AISI
HVOF Thermal HA, CoNiCrAlY, WC 70, -, 100 [83,84,124]
4340 SS
Al2 O3 -ZrO2 - yttria stabilized
zirconia (YSZ), Metco 447-
Plasma spray Thermal Alumina/Titania 87/13- Nicrome SS, steel, AISI 4140 steel -, 0.5–1, - [91,92,96]
80/20- Hastalloy G30,
TiC-NiCrBSi
HA, AA7075, Ni/Al, mixed
Cold spray Physical Ti-6Al-4V, Al 6061-T6, Al 6061 100–1000, 40–300, - [103,105,106]
Ni/Al/MoO3 , and Ni-clad Al
Zr-Cu12.3 Ni7.6 -Al3.5 , Ti, Ti,
Warm spray Physical 316L SS, steel, steel, carbon steel 400–1000, -, 400, 300 [108,110,111,125]
WC-Co
Arc wire spray Thermal MoS2 -TiC-Fe, Ti/Al Carbon steel, SUS 304 1000, - [112,113]
Table 4. Advantages and disadvantages of reliable coating processes.
Deposition Process Advantages Disadvantages Reference

Corrosion and wear resistance/thin film deposition is Requires a high vacuum/corrosion resistance is affected
PVD possible/adjustable mechanical, corrosion and aesthetic by abrasion/degradation control is challenging for [9,17,18]
properties polymer deposition applications
Corrosion and wear resistance/deposition of various
Requires ultra-high vacuum/requires heat resistant
CVD types of materials with different microstructures/works [24,25,30,31]
substrates/small amount of coating materials waste
with low and atmospheric pressures
High corrosion resistance and hardness/porous
MAO structure for biomedical applications/different scales of Mostly applicable to valve metals [33,35]
porosity through the thickness/
Decorative and low-corrosion/wear
ELD Works for conductive substrates [46,47]
applications/high-temperature applications
Various kinds of selective, graded material, and porous
EPD structure depositions/biomedical applications/wear Works for conductive substrates [53,54,59]
resistant
Cost effective/biomedical applications/providing
corrosion and ion release protection/multilayered Thickness control/slow rate of coating cycle/possibility
Sol–gel (thick) coating/high adhesion/ability to coat complex of coating failure during heat treatment on multilayered [66,67]
geometries/flexibility in the composition/no need of coating structures
conductive substrates
High density of coating layer and well substrate Requires a small range of powder size (5–60 µm) with a
HVOF adherence/works for non-conductive narrow size distribution/numerous process variable to [83–88]
substrates/corrosion and wear resistance change the coating structure/requires a heat source
High corrosion and wear resistance/high substrate A low-temperature process that is mostly used for
adherence/surface modification of engineering materials that cannot perform reactions in atmospheric
Plasma spray [92,93]
polymers, rubbers, metals, and fibers/anti-stick pressure to modify the surface of the substrate/requires
coatings a heat source
Limited operation range/mostly used for soft and hard
Simple and cheap method compared to the other metal substrates/low efficiency and reliability due to
Cold spray [102,103]
thermal spray methods low temperatures/not useful extremely harsh
environments
Applicable to materials with sensitivity to oxidization at Impurity complications/not useful extremely harsh
Warm spray [108,109]
high temperatures or heat sensitive materials environments
Internal surface coatings such as engine blocks/wear Limited to conductive wires and materials as the
Arc wire spray [79,113]
and corrosion resistant coating layer
Funding: This research received no external funding.

Conflicts of Interest: The authors of this work ensure that there is no conflict of interest by any means and the
study is not funded by any organization.
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On Coating Techniques for Surface Protection: A Review

Article in Journal of Manufacturing and Materials Processing · March 2019

Ben Fotovvati Navid Namdari

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Keywords: surface modification; sol–gel; thermal spray; vapor deposition

J. Manuf. Mater. Process. 2019, 3, 28; doi:10.3390/jmmp3010028 www.mdpi.com/journal/jmmp

2. Reliable Coating Methods

conductive π-conjugated polymers such as poly(2,5-thienylene) (PTh), and poly(pyridine-2-5-diyl)

2.4. Electrodeposition Coating

Figure 5. Schematic setup for electrodeposition of copper metal particles

Figure 6. Sketch of the electrophoretic deposition process

Table 1. Characteristics of electrodeposition techniques [61].

Table 2. Electrochemical corrosion measurements of different coating composition provided by

Figure 10. Schematic [98]..

2.6.4. Warm Spray Coating

2.6.4. Warm Spray Coating

2.6.5. Arc Wire Spray Coating

Table 3. Summary of coating processes and their specific feature.

Table 4. Advantages and disadvantages of reliable coating processes.

Deposition Process Advantages Disadvantages Reference

Funding: This research received no external funding.

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