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Materials Today: Proceedings 22 (2020) 1554–1562 www.materialstoday.com/proceedings

ICMMM 2019

A Critical Review on Nano structured Coatings for Alumina-Titania

(Al2O3-TiO2) Deposited by Air Plasma Spraying Process (APS)
Mohammed Thalib Basha Ga, Akella Srikantha, B.Venkateshwarlua,*
a
Research Scholar, Department of Manufacturing, School of Mechanical Engineering,
Vellore Institute of Technology, Vellore, Tamilnadu, 632014
a,
*Associate Professor, Department of Manufacturing, School of Mechanical Engineering,
Vellore Institute of Technology, Vellore, Tamilnadu, 632014

Abstract

The thick coatings obtained from nanostructured powders with fine layered microstructure are usually deposited using Air
Plasma Spraying process (APS). In APS, nitrogen or argon gas is used as primarily. Microstructural characteristics of coatings
for nanostructure powders are typically affected by the proportion of undissolved or partly melted zone (PM regions) present in
coatings microstructure. It is observed that volume portion of partly melted regions is seen to be very much smaller in coatings
obtained from nanostructurerd Al2O3-TiO2 powders deposited with nitrogen as compared to argon as the essential plasma gas.
Coatings acquired from agglomerated powders of nanostructured alumina-titania shown to qualify superior resistance to wear
over coatings by conventional powders. The Bi-modal representation of microstructures in nanostructured coatings with
homogeneous dispersion of partially melted areas in fully melted region are considered to be responsible for improved properties
of nanostructured coatings. This paper attempts to critically review the recent works done on atmospheric plasma sprayed
nanostructured Al2O3-TiO2 coatings deposited by either argon or nitrogen as primary gas.

© 2019 Elsevier Ltd. All rights reserved.

Peer-review under responsibility of the scientific committee of the 2nd International Conference on Materials Manufacturing and
Modelling, ICMMM – 2019.

Keywords: Air Plasma Spray; Nanostructured coatings; Plasma gas; Wear resistance; Conventional powders.

* Venkateshwaralu. Tel.: +91-9500646281.

E-mail address: venkateshwarlu.b@vit.ac.in, venkatsoft2004@gmail.com

2214-7853 © 2019 Elsevier Ltd. All rights reserved.

Peer-review under responsibility of the scientific committee of the 2nd International Conference on Materials Manufacturing and Modelling,
ICMMM – 2019.
 Mohammed Thalib Basha G. et al. / Materials Today: Proceedings 22 (2020) 1554–1562 1555

1. Foundation to APS process

The working principle of air plasma spraying process is shown in Figure 1. A DC (Direct Current) electric spark
is generated in between an annular copper anode and a tungsten tipped copper cathode. The both cathode and anode
are water cooled and separated by a small gap of a few mm. Ionizing gas such as argon, nitrogen, hydrogen or
helium is admitted into the annular space between the electrodes. In plasma spraying, argon and nitrogen are called
as primary plasma gases and hydrogen and helium are called as secondary plasma gases.introduction

Fig. 1. Schematic of Plasma Spraying Process [1]

1.1. Mechanism of Plasma Spraying

The plasma gas admitted into the annular space undergoes ionization in high temperature region created by the
DC electric arc and produces plasma. Ionization of gas occurs from collision of electrons in the form of arc. Small
amounts (5-10%) of hydrogen or helium are typically added to the primary plasma gas, for example, argon or
nitrogen, when high gas thermal conductivity is desired for better melting of materials like ceramics. The Plasma
that is formed in the nozzle is highly unstable and it recombines to form a neutral gas again and thus releases large
thermal energy [2]. Coating material in powder form suspended in the form of carrier gas which is to be injected into
the plasma jet using powder feeder system in a metered quantity. The injected powders either melt fully or partially,
or remain unmelted depending on the trajectory they take within the plasma jet. While powder particles that remain
within the plasma jet core melt fully, those on the outer periphery melt partially or remain unmelted. Upon entering
the plasma jet, the powder particles again gain the momentum from plasma gas and rush towards the target which is
known as the substrate to form a thin layer on it. Thus the consecutive layers are deposited onto the earlier one and
the coatings build up layer by layer to the desired thickness [3].

1.2 Crack Growth resistance of Nanostructured Plasma Sprayed Alumina-Titania Coatings

The coatings obtained from Air Plasma Spray processed Alumina-Titania powders are widely utilized in various
applications like faucets, piston rods, seals for pumps, engine parts, rocket nozzles, embedded circuits vacuum tube
envelopes, shields for guided missiles, railroad elements, etc., [4] since it possess resistance to extreme wear
conditions, as well as resistance to thermal shock, oxidation and warming deterioration resistance and electrical
protection [5]. Alumina-Titania coatings can also adhere easily with the bond of metallic coats so that it can
withstand wear and solid particle erosion and possess superior hardness value and chemical constancy even at raised
temperatures [6].
1556 Mohammed Thalib Basha G. et al. / Materials Today: Proceedings 22 (2020) 1554–1562

Fig.2. Comparison of cracks arising from Vicker’s indentation for 500gf in alumina based systems. (a) Long Cracks
generate in crushed alumina; (b) Cracks of moderate length in agglomerated alumina and (c) Shortest cracks in nano
alumina-titania [10]

Several explanations have been given in literature to explain the improved crack growth resistance of
nanostructured thermally sprayed coatings obtained from agglomerated powders over those from corresponding
conventional powders and those are : (i) Enhanced splat-to-splat cohesion in nanostructured coatings obtained from
composite agglomerated powders, for example, alumina-13wt% titania, due to lower melting point of agglomerated
powders, from intimate mixing of multiple phases, which in turn leads to lower viscosity and better wetting of splats
on already solidified coatings [7], (ii) Crack deflection and arrest at interfaces between fully and partially melted
regions [8], (iii) Enhancement of fracture toughness of partially melted phases due to residual stress field arising
from difference in coefficients of thermal expansion and thereby difference in shrinkage during solidification of fully
and partially melted phases and (iv) Crack arrest within the partially/unmelted regions. Scanning Electron
Microscope (SEM) images showing different crack arrest mechanisms for coatings obtained from nanostructured
powders are shown in Figure .2. The presence of bi-modal microstructure in coatings obtained from nanostructured
powders is seen to be responsible for their improved crack growth resistance [9, 10].

2. Sample preparation and Experimentation

Generally, in all the coating instances of air plasma process, coatings were deposited over steel surface of
standard dimension of 65X55X5 mm size. The surface grinder to be utilized to grind down the uppermost and
bottom faces of surface to vanish the oxide layers and create even surfaces of a maximum surface roughness of
nearly 0.1microns. Ahead the procedure of thermal spraying process, the specimens were sand blasted using alumina
grits with standard pressure and stand-off distance. This blasting process too helps in vanishing the oxide region
which forms at the time between grinding and blasting. After grit blasting, the substrate is to be ultrasonically
cleaned mostly in iso-propanol bath to take out smudge and unwanted scrap present in the specimen. Next,
preheating is done to remove grease, oily substance, water vapor, etc. if any present on the substrate surface.
In most of the works, coatings of around 250-350 microns thick were deposited using air plasma gun. Argon and
helium are utilized as essential and auxiliary plasma gases respectively. For remaining analysis, specimens with
dimensions 10x5x5 mm magnitude are cut off from the coating samples and characterized by SEM, X-Ray
diffraction, Vicker’s micro hardness tester and Porosity test, etc. For tribological characterization, the samples are
prepared according to the standard dimensions based on the size of the disc of pin on disc tribometer and multiple
wear tests are performed on coated samples at different load and speed conditions [11].
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3. Microstructural and Tribological Characterization

The microstructure of nanostructured alumina-13wt% titania coatings showing partly melted area (PM regions) is
shown in Fig.3 (a). It was found that nanostructured coatings exhibit extreme hardness, resistance to wear and
fatigue intensity than their conventional counterparts. The fatigue test carried out by Rotating beam of AISI 1020
(0.2% Carbon) steel specimen coated with conventional and nanostructured alumina-13wt% titania coatings of 50
Hz showed that fatigue life of steel specimen with nanostructured alumina-titania coatings were around two-three
times high as compared to that of coatings obtained from conventional powders and around 4 times higher than that
of specimen without any coatings (See Fig.3b). The growth in fatigue intensity of specimen coatings with
nanostructured is attributed to higher resistance to crack extension and interfacial toughness of nanostructured
coatings [12].

Fig.3. (a) Morphology of Transversal section of nanostructured Alumina-13weight%Titania Coatings; (b) Fatigue period
distributions of coated and uncoated samples

3.1. Effect of bi-modal microstructure

The resistance for cracks due to indentation of plasma sprayed Al2O3-13wt%TiO2 nanostructured coatings
containing bi-modal microstructure is determined and compared with conventional coatings having same
composition (i.e. Metco-130 coatings). Metco 130 coatings have only fully melted alumina splats, lengthy cracks
initiated at notch corners and propagated on boundaries where splats are present in their microstructure. As a result,
nanostructured coatings were the combination of bi-modal microstructures i.e.,completely melted splat part and
partly melted particulate part, and these partly melted particulate regions are served to entrap and deviate the cracks
near splat boundaries. Interfaces between full melted regions and partly melted regions provides an extra crack
arresting mechanisms. By optimizing these conditions, the toughening processes produced nearly 100%
improvement in crack growth resistance. A microstructure comprises 15-20% of partly melted(PM) particulate
regions could be consistently limited by varying temperature of plasma gas, was found to be the optimal one [8].
The partly melted area comprises of liquid phase sintering i.e., (3D net like structure, Al2O3-loaded submicrons
enclosed in TiO2 matrix) and solid-phase sintering part (comprises nano particles in unmelted condition). It was
observed that particles which attain in the range 1840 ℃ melting temperature of TiO2, and 2045 ℃ melting
temperature of Al2O3, undergoes phase of liquid sintering, meanwhile those that reach below 1840℃ undergoes
phase of solid sintering. Commencement of liquid and solid phases sintered parts in partly melted portions are
responded to the melting temperature deviation of Al2O3 and TiO2 [13].It can be noted that the conventional coatings
consist of only fully melted(FM) regions lamellar-structure in their microstructure.
1558 Mohammed Thalib Basha G. et al. / Materials Today: Proceedings 22 (2020) 1554–1562

3.2. Wear Characterization of conventional and nanostructured coatings

The process of characterization of wear due to sliding of air plasma sprayed(APS) Alumina(Al2O3)-
Titania(TiO2) coatings are determined using wear tests on pin-on-disc tribometer. It was observed that the friction
co-efficient increases by increasing the load applied and the velocity range due to sliding. Remarkable cracking
phenomenon and spallation due to wear were found for conventional coatings, meanwhile minimal localised
spallation were obtained for the coatings with nanostructured powders as shown in Figure. 4 [14]. It was also
observed that the coefficient of friction increases with spacing between the flame produced by plasma and the
powder injection location. In some earlier studies the wear characterstics of alumina-titania coatings are also related
to with spraying parameters such as rate of flow of primary gas and secondary gas, rate of flow of carrier gas ,
powder injection spacing distance etc., and observed that there is a joint outcome of spraying temperature and
resistance for wear characteristics of these Alumina-Titania coatings [15].Fretting wear examination were
performed for Alumina(Al2O3)-Titania(TiO2) coatings by 52100 steel balls. Coatings with nanostructured powders
were found to possess more improved resistance for fretting wear as compared to coatings with conventional
powders due to the impression of grains with nano-sized structures, minimized structures of amorphous and
lamellar phases. Meanwhile there are no pattern for the propagation of cracks was seen in coatings with
nanostructured powders, cracks due to fretting were visible to propagate on the boundaries of splats in the coatings
with conventional powders. During fretting wear tests on the coatings with nanostructured powders, a transferal of
layer of the iron oxide were found on the worn-out surface of the coatings. The friction co-efficient was also
measured during tests and it is in the range of 0.7-0.9 [16].

Fig.4. Results after the cup tests for (a) Conventional; (b) Coatings obtained from nanostructured powders

The examination for dry sliding wear of coatings with nanosuctured and conventional Al2O3-13wt%TiO2
powders was investigated. It was found that coatings obtained from nanostructured powders possess increased
resistance wear at all loading conditions. Transformation from moderate to intense wear was found for coatings
obtained from nanostructured and conventional powders. Nevertheless, the hypercritical pressure at which
transformation appeared was higher for coatings obtained from nanostructured as compared to coatings from
conventional powders. The propagation of cracks was controlled by the PM regions during wear of coatings
obtained from nanostructured powders. Also, the propagation of cracks along the boundaries of splats at lower loads
whereas at higher loads the cracks penetrates through the splats. It was also observed that at lower loads, the cracks
are grabbed and deviated by initial grade of microstructure which starts to be effective and the cracks are then
 Mohammed Thalib Basha G. et al. / Materials Today: Proceedings 22 (2020) 1554–1562 1559

distracted by the nanoparticles present in the partial melted zones. The deflection of these cracks is responsible for
the toughening effect and improvement in wear resistance of coatings obtained from nanostructured powders[17].
The resistance for the wear due to abrasion of coatings obtained from nanostructured Al2O3-13wt%TiO2+CeO2 and
Al2O3-13wt%TiO2 +CeO2+ZrO2,Al2O3-13wt%TiO2 powders was found to be more superior to that of coatings
obtained from conventional powders. Among all the compositions used to obtain coatings from nanostructured
coatings, the lowest volume of wear rate for coatings containing Cerium Oxide(CeO2) and Zirconium Oxide(ZrO2).
While no correlation was observed between wear volume and coating hardness, wear volume was seen to be directly
proportional to the crack length in indentation tests. The results of XRD analysis of conventional and nanostructured
coatings before and after the wear tests showed that there is a phase change of gamma Al2O3 to alpha Al2O3. The
phase transformation was particularly significant in nanosuctured coatings containing CeO2 and ZrO2 [18].
Pin-on-disc(POD) test and dry sand steel wheel tests were performed to determine resistance to wear for three air
plasma sprayed ceramic coatings of alumina, alumina-13wt% titania and Cr2O3 which are hard and brittle in nature.
In all these coatings, dry particles abrasion occurring through splats detachment was observed. Alumina coatings
showed the highest wear resistance among three coatings. These coatings were in fact seen to perform better than
coatings obtained from HVOF process and Chromium electroplated coatings when the less number of wheel
rotations were considered. While performing pin-on-disc tests, no coating composition possess loss due to wear
against 100Cr6 ball which exhibits low hardness level. While using alumina balls, alumina and alumina-titania
coatings showed higher rates of wear and friction coefficients because of chemical relationship and
Cr2O3(Chromium Oxide) coatings exhibits improved resistance to wear, lesser coefficient of friction and lesser wear
on the coated sample [19]. The resistance to wear due to erosion of the alumina and chromium oxide composite
coatings was examined by a recent type of test called as solid particle impact test. The addition of Cr2O2 promotes to
the compaction of coatings that is strengthened through particle solid solutioning. This composite coating also
provides excellent wear resistance and lower erosion depth as compared to pure alumina coatings [20].

3.3 Studies on Mechanical Properties of Conventional and Nanostructured Alumina-Titania coatings

The conventional and nanostructured Nickel-Chromium-Alumina-Yttria-Molybdenum-Silver coatings were

deposited using air plasma spraying. The coatings obtained from nanostructured composite powders showed
minimum defects, lesser porosity and more smaller wedged structured grains as compared to that of coatings
obtained from conventional powders. The coatings obtained from nanostructured composite powders also have
maximum micro hardness and strength of adhesion. It is observed that the sliding activity in wear tests raise the
tribo-chemical reaction of molybdenum, nickel and silver over the wear-out surfaces of coatings [21].
The two types of coatings viz., Al2O3-40 wt%TiO2 with Nickel- Alumina splats termed as AT40 and Al2O3-40
wt%TiO2 with Nickel- Alumina termed as MAT 40 fabricated by using Air Plasma Spray process. The fracture
toughness of MAT 40 coatings system is greater than AT40 due to the modification of Nickel-Alumina splats, that is
responsible for releasing bending stress. The crack is to be distracted when very small sized Ni-Al splats were met
and it was observed that in ceramic zonal cracks propagate on the boundaries of columnar grains [22]. The
performance of three coatings obtained from nanostructured powders Al2O3 mixed with ZrO2 in different
percentages of 35%, 40%, 45% was studied. It was found that coatings obtained from alumina-40% zirconium oxide
have shown highest density, low porosity and few micro cracks. The micro hardness of these coatings was observed
to be decreasing by decreasing Al2O3 content [23].The coatings obtained from nanostructured Al2O3-TiO2 powders
over austenitic stainless steel substrate using Air Plasma Spraying process. The thermal treatment was found to be
an effective process for generating extremely sinterable feedstock made of nanostructured powders to yield coatings
with low porosity. It was observed that the amount of semi-molten environment can be controlled by modifying the
characteristics of feedstock [24].
The characterstics of suspension plasma sprayed nanostructured Al2O3-TiO2 coatings were evaluated and it was
observed that alumina is present in the coatings in the form of gamma alumina and corundum. It was also observed
that partly melted (PM) zones present in the microstructure of these coatings are similar to that of PM zones present
in the APS sprayed coatings. Formation of aluminum titanate was also observed in their microstructure and this is
due to reaction of titania with alumina during spraying process [25].
1560 Mohammed Thalib Basha G. et al. / Materials Today: Proceedings 22 (2020) 1554–1562

The composite consists of Alumina-Zirconia coating systems were prepared by Supension Plasma
Spraying(SPS), to attain compact and structure with cohesive property. Various parameters such as less spraying
distance, less nozzle diameter, and very low solid mass ratio leads to the decreasing in stack density. Microstructure
of coating indicates the presence of high alpha-alumina [26].
The rate of wear and mechanical characterization of Al2O3-43wt%TiO2(AT-43) and Al2O3-13wt%TiO2(AT-13)
acquired by the thermal spraying process such as Air plasma spraying and Flame spraying process. The primary
phase established in AT-13 coating system were gamma Al2O3 with alpha Al2O3 which provides improved
mechanical properties to the coatings whereas AT-43 coatings possess Al2TiO5 and Al6TiO13 phases, and both the
phases are brittle in nature and has poor mechanical properties. Both flame and APS process shows similar wear
rates, porosity percentage and hardness [27].
Al2O3-40wt%TiO2(AT 40) coating process was carried out by Air Plasma Spraying. Phase distribution, micro-
hardness, wear mechanisms and spraying conditions were investigated. The results showed that the already existing
morphology of surface mainly evaluates the distribution of phases. Al2TiO5 and gamma-Al2O3 are the important
phases in the coatings. The highest micro-hardness was 1126.11VHN( Vicker’s Hardness Number) and wear rate at
that point were readed as 0.0387 mg/Nm which is the minimal weight loss calculated among all the samples
examined. The mechanism for wear is mainly due to the scratches due to abrasion. The lamellar distribution of
phases reduces the number of surface defects, increases the hardness and also spraying condition affects the
distribution of phases [28].

3.4. Effect of deposition on carbon fibers

The coatings obtained from nanostructured Al2O3-13wt%TiO2 powders were deposited on T700 carbon
fibers/epoxy simplex plate using Air Plasma Spraying process. The bonding nature and hardness of the coatings
obtained from nanostructured ceramic oxide increases and then starts dropping by increasing the current intensity.
Also, the hardness and bonding strength peak at the current of 650 A [29].

3.5. Impact of adding graphite to the powders

The outcome of adding graphite to Al2O3-13wt%TiO2 coatings for the analysis of wear due to friction as well as
abrasion. An effort was carried out to examine the consequences of gamma-Al2O3 translation over the coated surface
where the wear due to abrasion occurs. The X-ray Photo electron Spectroscopy(XPS) and Debris analysis for wear
measurement provides significant data about tribo-chemical reactions. These data are very much useful to
interconnect the wear of the coatings due to abrasion and friction. The decrement in coefficient of friction for the
coatings with mixture of Nickel and Graphite to Al2O3-TiO2 system as compared to that of Al2O3-13wt%TiO2
system. This is mainly due to the presence of a self-lubricating film which is made up of graphite. The
advantageous result of adding graphite to Al2O3-13wt%TiO2 coating system is that the wear due to abrasion can be
reduced. The wear due to abrasion mainly depends on mechanical and microstructural properties of coatings
obtained and the distribution of particles. From the possibility for contacting the coated surface, the wear rate due to
abrasion can be easily predicted and can be located the failure zone of coatings [30].

3.6. Effect of heat treatment on Alumina-Titania coatings

The phase composing the chosen amalgamated and rough Al2O3-40%TiO2 raw powder to be successfully
modified by the process called normalizing(process of heating and cooling in air). During this process, there should
not be any change in the distribution of particle size and the ability to processing by Air Plasma Spraying process.
The morphology of powder shows some changes only when the coating powder is supposed to heated upto 1500℃.
The feedstock powder contains alumina and titania and both these elements not showing any homogeneity in the
distribution of particles. The particle of alumina also shows titania as an impurity. To overcome the effect of uneven
distribution Al2O3 and TiO2 particles, the powder is to be heated to 1150℃, so that the powder can be prepared with
the content >50wt% Al2TiO5. The even distribution of particles and the presence of less impurity in the feedstock
powder improves the characterization of the powders as well as the coatings obtained from that powders[31].
 Mohammed Thalib Basha G. et al. / Materials Today: Proceedings 22 (2020) 1554–1562 1561

4. Summary

Nanostructured powders provides constant, homogeneous flow of powder than that of conventional powders
which possess angular and block-like structures. The ability of the nanostructured powders to flow freely is mainly
due to the morphology of powders i.e., spherical. The microstructure of the coatings obtained from nanostructured
powders possess bi-modal(partly melted portion in the completely melted zone). Whereas, no partly melted zone is
obtained in the coatings obtained from conventional powders. There are various spraying parameters which are
responsible for the percentage of partly melted zone present in the coatings. Anyhow, the partial melted zone
percentage was very less for the coatings obtained from nitrogen gas as compared to coatings obtained by argon gas.
The proportion of alpha-alumina present in the coatings obtained from nanostructured powders was found to be
mainly subjected on the selection of gas used for plasma. The presence of alpha-alumina in the coatings decide the
resistance to high temperature. The proportion of alpha-alumina present in the coatings obtained from
nanostructured powders was superior as compare to the coatings obtained from conventional powders. Also, it
should be noted that both type of coatings uses argon to be primary gas. On the whole, it can be concluded that
nanostructured Al2O3-TiO2 coatings are supposed to provide optimized mechanical and tribological properties as
compared to conventional Al2O3-TiO2 coatings. Pre heating of nano sized powders also gives better performance in
phase analysis. Various methods and different compositions were performed to analyze the consequences of air
plasma spraying parameters on the coating characteristics.

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