J Therm Spray Tech
https://doi.org/10.1007/s11666-020-01033-6
PEER REVIEWED
High-Performance Al2O3 Coating by Hybrid-LVOF
(Low-Velocity Oxyfuel) Process
Satish Tailor1 • Nitesh Vashishtha1 • Ankur Modi1 • S. C. Modi1
Submitted: 23 October 2019 / in revised form: 14 March 2020
Ó ASM International 2020
Abstract Plasma spraying is now a standard coating pro-
cess to deposit ceramic coatings for applications in auto-
motive, aviation, medical and health care and others. This
study deals with a hybrid thermal spray technique to
deposit ceramic coatings. This technique named ‘‘hybrid-
LVOF’’ (low-velocity oxyfuel) makes it possible to deposit
uniform thin or thick ceramic coatings on metallic or
ceramic substrates. In this work, the microstructural and
mechanical properties of Al2O3 coating deposited by
hybrid-LVOF were compared with those of Al2O3 coating
deposited by the conventional plasma spray technique. The
Rietveld refinement of XRD patterns was used to quantify
the a-Al2O3 and c-Al2O3 coating content. Hybrid-LVOF
as-sprayed coatings have a smoother surface, lower
porosity (2–3%), higher hardness and better adhesion
strength than conventional plasma-sprayed coatings. The
hybrid-LVOF coatings also exhibit better fracture tough-
ness probably because of a high inter-splat bonding and
low porosity.
Keywords Al2O3  ceramic coating  hybrid-LVOF 
mechanical properties  phase transformation  plasma
spraying
& Satish Tailor
dr.saty@yahoo.in
1
Metallizing Equipment Company Pvt. Ltd., E-101, MIA
Phase-II Basni, Jodhpur, India
Introduction
Plasma spraying is a versatile coating technique widely
used to deposit Al2O3 ceramic coatings for anti-wear, anti-
corrosion and electrical insulation application due to the
high hardness and high temperature stability (up to
1100 °C) of alumina. The coatings are used on many
industrial parts such as rolls, shafts, plunger, turbine blade,
rocket nozzle, pump seals and steam valve spindle (Ref 1-
3). Flame spraying, high-velocity oxyfuel (HVOF) spray-
ing and plasma spraying can be used to deposit ceramic-
based coatings (Ref 1, 4, 5). The important parameters that
influence the microstructural and mechanical properties of
thermal sprayed coatings are the velocity, temperature and
molten state of the impacting particles as well as the sub-
strate roughness, oxidation, cleanliness and temperature
during the coating process. Plasma-sprayed coatings gen-
erally exhibit a rather high porosity (4-12%) that affects
their structural and mechanical properties (Ref 6, 7).
The crystallographic phase transformation of feedstock
material during spraying can also play a crucial role in
controlling the alumina coating properties and perfor-
mances. Plasma-sprayed Al2O3 coatings from a-Al2O3
powder generally contain the metastable c-Al2O3 phase
with a small percentage of the a-Al2O3 stable phase (Ref
8).c-Al2O3 nucleates in preference to a-Al2O3 because of a
lower nucleation energy, and the cooling rate after solidi-
fication is sufficiently rapid(106-108 K/) to prevent trans-
formation to d-Al2O3 or a-Al2O3 (Ref 9). c-Al2O3 to a-
Al2O3 phase transformation occurred at 1100 °C which is
lower than the melting temperature of Al2O3 (2050 °C)
(Ref 10). High a-Al2O3 content in as-sprayed Al2O3
coating was reported to be beneficial for electrical insula-
tion and wear resistance properties (Ref 10), and this may
123

be explained by the hexagonal close-packed-structured a-
Al2O3 in comparison with the cubic structured c-Al2O3.
Some researchers have attempted to get a higher a-
Al2O3 phase content in coatings by controlling the depo-
sition parameters, spraying technique, cooling rate and
feedstock coating material (Ref 6, 11-13), e.g., the c phase
content of the coating increases with an increase in the
plasma torch power because of a better melting of the
feedstock powder (Ref 14), while the doping of alumina
with Cr2O3, Y2O3 and CeO2 results in a significant stabi-
lization of a-Al2O3 and improvement in the thermal con-
ductivity and mechanical properties of coatings (Ref
15, 16). For instance, a significant change was observed in
the coating alpha to gamma mass ratio from 0.08 to 0.53
for Al2O3 powder doped with 18%Y2O3 (Ref 15) and the
coating heat treatment above 1100 °C led to the complete
transformation of the c to a phase. However, such heat
treatment is not recommended due to a rise in thermal and
mechanical stress and also volume change (the density of
the a-phase and c-phase is 3980 kg/m3 and 3600 kg/m3,
respectively) that can cause cracking and fragmentation of
coating (Ref 8, 17). Improved coating densification and
mechanical properties thanks to a laser treatment that
induced the c to a phase transformation were also reported
(Ref 18).
In this study, Al2O3 coatings were deposited by a newly
developed thermal spray hardware for the improvement of
their structural and mechanical properties. This technology,
named hybrid-LVOF, is designed and manufactured by
Metallizing Equipment Company Pvt. Ltd. (MECPL)
India. It is a cost-effective solution to spray ceramic
coatings. A comprehensive comparison of structural and
mechanical properties of plasma-sprayed and hybrid-
LVOF-sprayed Al2O3 coating is discussed. Other motiva-
tion was to achieve a higher a phase content in as-sprayed
Al2O3 coating compared to plasma-sprayed Al2O3 coating.
Experimental
Materials
Commercially available Al2O3 powder (Amperit 740.000,
H. C. Starck GmbH) was used as feedstock material for
coating deposition. The powder particle morphology is
shown in Fig. 1. The particle size ranges between 10 and
30 lm. Low-carbon steel plates of 50 9 50 9 5 mm3 were
used as substrate material.
Coating Manufacturing
The coatings were deposited i) using an atmospheric
plasma spray (APS) system MEC Plasma PSC:50/100,
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J Therm Spray Tech
Fig. 1 SEM micrograph of Al2O3 feedstock powder
Make MECPL, India) with a M-F4 plasma gun (Make
MECPL, India) and ii) with the newly developed hybrid-
LVOF technology (Patent applied; Make MECPL, India).
For the hybrid-LVOF hardware, a number of experiments
were first conducted to determine the optimum design of
the gun nozzle and spray parameters.
All substrates were blasted before coating deposition
using a pressure-blasting machine (M/C- SU-9182 –,
MECPL, India) with brown alumina grits of 60 lm in
diameter. After grit blasting, the substrates were cleaned
with ethanol and then kept inside an oven at 100 8C for
5 min. The average surface roughness after blasting was 6
± 2 lm.
The optimized spraying parameters for plasma spraying
were a plasma-forming gas mixture of argon (38 slpm) and
hydrogen (9 slpm), arc current of 575 A, carrier gas flow
rate of 3.50 slpm, powder feed rate of 30 g/min, spray
distance of 65 mm and spray angle of 908. The mean arc
voltage was 96 V. For the hybrid-LVOF process, the
spraying parameters were an oxygen flow rate of 60 slpm,
Acetylene of 70 slpm, powder feed rate of 50 g/min, spray
distance of 80 mm and spray angle of 908. Both processes
used a 6-axis robot (Kuka, Germany) to achieve uniform
pass thickness. Air jets were used to cool down the sub-
strate below 100 8C and remove the weakly bonded par-
ticles from the coating surface. The average Al2O3 coating
thickness was 250 lm in both cases.
Hybrid-LVOF Process and Procedures
This new technology is mainly designed for ceramic
coatings. It differs from plasma spraying in term of heat
source and particle velocity. It is based on a hybrid con-
cept, which results in a lower particle temperature in
comparison with the plasma spray process but higher in
comparison with the HVOF process, i.e., sufficient
J Therm Spray Tech
temperature to melt the ceramic particles. To increase the
flame temperature, some changes were made in the HVOF
torch design by adding a spray nozzle. The latter helps to
get sufficient temperature and high particle velocity. A
cross-sectional view of the hybrid-LVOF torch is shown in
Fig. 2. With this technique, the alumina particle velocities
ranged between 200 and 300 m/s, while they roughly range
between 500 and 600 m/s in HVOF spraying and between
100 and 200 m/s in plasma spraying. In addition, the flame
temperature in hybrid-LVOF spraying is much lower than
that of a plasma jet but slightly higher than a HVOF flame.
The alumina particle velocity and temperature were
measured by using the SprayWatch (Osier, Finland) diag-
nostic system. The particle temperature in hybrid-LVOF
Fig. 2 Schematic of the concept of H-LVOF process
Fig. 3 Cross sections and top
morphologies of as-sprayed
Al2O3 coating, (a, b) Plasma
sprayed; (c, d) H-LVOF sprayed
spraying was in the range of 2300–3000 °C which makes it
suitable for depositing ceramic coatings.
Hybrid-LVOF spraying is a lower power spray tech-
nique and a cost-effective method as compared to plasma
and HVOF spraying techniques. It results in lower coating
cost than plasma spraying because only fuel gases are used.
In addition, the equipment cost is lower (about USD
100,000). Compared to plasma spraying, the radiation and
noise level is much lower. The plasma and hybrid-LVOF,
noise intensity was measured with the help of a sound level
meter (SLM 200 HF, Excellent Industrial Instruments
Chennai, India) and was found to be 140 decibels and 110
decibels, respectively.
The Occupational Safety and Health Administration
(OSHA) has a standard for nonionizing radiation restricts
electromagnetic radiation to only that portion of the spec-
trum defined as radio frequency. Thermal spray processes,
such as plasma and arc spray, produce UV light. Safety
rules applicable to thermal spray can be found in the OSHA
standard Subpart Q-Welding, Cutting, and Brazing of
29CFR 1910. Plasma spray process produces much a
brighter light between 280 and 220 nm, also called the UV-
C region. It also generates ozone. The cornea of the eye
easily absorbs the UV from these regions, leading to a
condition called flash burn after prolonged exposure. Eyes
can be damaged without discomfort during exposure.
Repeated exposure to UV may decrease skin elasticity.
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(a)
(b)
Fig. 4 Cross sections of as-sprayed Al2O3 coatings at higher
magnification, (a) plasma sprayed and (b) H-LVOF sprayed
This can give the appearance of premature aging and can
lead to a higher risk of skin cancer, whereas combustion
spray processes (HVOF/flame) do not produce such high-
intense UV radiations.
Powder and Coating Characterization
The morphology of feedstock powder and microstructure
of coatings were observed using scanning electron micro-
scopy (SEM: Carl Zeiss Evo18, Germany). Energy-dis-
persive spectroscopy (Oxford, EDS) was used to check
their elemental chemical compositions. For microstructural
analysis, the coated samples were cross-sectioned, mounted
and polished up to 1 lm diamond suspension. X-ray
diffraction (XRD) method (PANalytical Empyrean Series
2, Netherlands) was used to analyze the phases present in
powder and coatings. XRD was operated at 45 kV and
40 mA with Cu-Ka radiation of wavelength 1.54059 Å.
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The XRD patterns were measured with a step size of 0.018
and dwell time of 0.5 s for 2h ranging between 20° and
90°. The residual stresses were determined with a x-ray
diffraction method. c-Al2O3 phase with a 2h peak position
of 45.73° was selected in residual stress calculations of
both plasma and hybrid-LVOF-sprayed coatings. QSMIAS
4.0 Metallurgical Image Analysis System (Make: M/s.
Qualitech Systems, India) was used to quantify the porosity
present in coatings as per ASTM B-276.
Dielectric strength measurements were taken using
TuR-WPT 0.8/65–GPT 3/80 (Veb Transformatorenwerk,
Germany) dielectric strength measurement kit. The
dielectric strength measurement kit was operated with a Ø
6 mm rod which supplied a 50 Hz alternating current (AC)
to the samples. The sample dimension was 50 9 25 mm2.
The steel substrate served as one electrode, and the second
rod electrode was placed to the coatings surface. All the
edges of the samples were covered with vinyl polysiloxane
to avoid surface discharges that usually occur below the
breakdown voltage between the electrode and steel sub-
strate. All the samples were dried in a furnace at 70 °C for
12 h prior to the test to get rid of the moisture content in
coating. The applied voltage was increased in steps of
500 V/s until the sample underwent breakdown. The
dielectric breakdown was confirmed using the character-
istic collapsing/ decrease in the voltage with a corre-
sponding increase in the current. Since the dielectric
strength is defined as the breakdown voltage divided by the
coatings thickness, it was computed from the average of
nine breakdown voltage measurements.
Mechanical Properties
The microhardness was examined with a Vickers
microindenture (SHIMADZU HMV-G-21ST, Japan) on
polished cross section with an applied normal load of 300 g
for all coatings. The reported value corresponded to an
average of 10 readings for each coating. The surface
roughness of the as-sprayed coatings was measured using a
Surface Roughness Tester (Mitutoyo Model- SJ-210,
Japan). Each coated sample was measured at five random
locations with the average and standard deviation of the Ra
values being quoted as per the ISO 4287:2015 standard.
For coating adhesion strength measurement, three cylin-
drical samples 25.4 mm in diameter and 50 mm in length
were prepared (thickness of 380 lm) as per the ASTM C-
633 standard. The adhesion bond strength test of the coated
samples was measured using Universal Testing Machine
(Model: Instron, Digital tensile bond testing machine
50 kN, USA) having a tensile load with transverse speed
ranging from 0.8 to 1.3 mm/minute. Coating’s fracture
toughness was estimated as per Vickers indentation pro-
cedure on polished cross section of coatings using a 5 N
J Therm Spray Tech

Fig. 5 XRD patterns of Al2O3 (a) feedstock powder, (b) plasma-sprayed coatings and (c) H-LVOF-sprayed coatings

load. The equation used in fracture toughness (KIC) cal- LVOF spraying are shown in Fig. 3a, b, c and d, respec-
culation is given below (Ref 19); tively. The porosity and average roughness of the plasma-
  sprayed coatings were 5.41 ± 0.52% and
KIC ¼ 0:079 P=a3=2 logð4:5a=cÞ ðEq 1Þ 7.47 ± 1.2% lm, respectively, while that of the hybrid-
LVOF coating were 2.42 ± 0.61% and 2.89 ± 0.5% lm,
where P is the applied indentation load, c is the crack
respectively. The analysis of the top morphologies of as-
length from the center of the indent, and a is the half
sprayed coatings showed that both coatings have porosities
diagonal length. The average of five readings along with
but different as-sprayed texture.
standard deviation is reported.
From Fig. 4, it can be seen that, in the conditions of this
study, the plasma-sprayed (Fig. 4a) coating has bigger
splats, weaker splat interfaces and higher porosity than the
Results and Discussion
hybrid-LVOF-sprayed coating. These observations are
consistent with that reported in previous studies on alumina
Coating Microstructures
plasma-sprayed coatings (Ref 20, 21). In the new process,
the higher kinetic energy helps into deformation and
The top morphology and microstructures of as-sprayed
spreading of the molten and/or partially molten particles
Al2O3 coatings deposited by plasma spraying and hybrid-
onto the substrate to form a denser coating (Fig. 4b). The

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20 μm
(a)
20 μm
(b)
Fig. 6 SEM micrograph of Vickers indentation for fracture tough-
ness calculation of as-sprayed Al2O3 coatings, (a) plasma sprayed and
(b) H-LVOF sprayed
thermal and kinetic energy of the molten or partially
molten powder particles controls to a large extent the splat
formation and coating buildup (Ref 11). The plasma-
sprayed Al2O3 coating revealed fine cracks at splats
interface shown in Fig. 4a with arrows, while the hybrid-
LVOF-sprayed coating is free from any such kind of
cracks. SEM micrograph of the plasma-sprayed coating
(Fig. 4a) also showed some non-melted particles, which
could be detrimental for tribological applications. A fine
intra-splat microstructure can be seen in the hybrid-LVOF-
sprayed coating.
Phase Transformation in As-sprayed Coatings
The initial phases present in the Al2O3 feedstock powder
determined by XRD were indexed as shown in Fig. 5a. The
diffraction pattern confirmed that only the a-Al2O3 phase is
present in the powder. Figure 5b and c shows the XRD
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patterns of the as-deposited plasma and hybrid-LVOF-
sprayed coatings, respectively. Both coatings contain c-
Al2O3 and a-Al2O3 phase. The coating c and a phase
content depends on the melting state of the impacting
particles that in turn, depends on the flame heat enthalpy
and particle residence time in the hot jet. The Rietveld
refinement of XRD patterns showed that the alpha to
gamma phase ratio was 0.081 for the plasma-sprayed
coating and 0.919 for the hybrid-LVOF-sprayed coating.
This could be attributed to the lower flame heat enthalpy in
hybrid-LVOF: a less amount of a to c phase transformation
took place during the spray process.
Porosity, Hardness and Fracture Toughness
Figure 3 and 4 shows a clear distinction in the porosity
(pore size and content) of the plasma-sprayed and hybrid-
LVOF-sprayed coatings: the former contained larger pores
(average pore size of 1.4 ± 0.7 lm) in comparison with
the hybrid-LVOF-sprayed coating (pore size of 1.0 ± 0.4).
The mean porosity was 5.4 ± 0.5 and 2.4 ± 0.6% for the
plasma-sprayed and hybrid-LVOF-sprayed coatings,
respectively. The lower porosity of the latter can result in
an improvement of mechanical properties of coating.
Al2O3 coatings are widely used as wear-resistant coatings.
Hardness and fracture toughness are two important prop-
erties that decide the mechanical performance of a coating
system. In this work, the measured average Vickers
microhardness was 712 ± 80 and 795 ± 20 HV for the
plasma-sprayed and hybrid-LVOF-sprayed coatings,
respectively. The higher hardness of the hybrid-LVOF-
sprayed coating results from the higher content of a-Al2O3
and lower porosity. Also, the low average deviation in the
hardness of hybrid-LVOF-sprayed coating reflects the
better microstructural homogeneity of the coating.
The e high particle velocity and good melting of powder
particles in the hybrid-LVOF process led to the formation
of good intra-splat bonding. The high impact velocity of
molten droplets caused a better deformation of the
impacting particles, whereas in the plasma process the
particle velocity is lower. A correlation between the coat-
ing porosity and mechanical properties can be expressed by
the following equation (Ref 22)
S ¼ SO expðbPÞ ðEq 2Þ
where S represents the fracture toughness for a material of
porosity P and SO the same mechanical property for a
porosity-free material, b is a constant. The porosity present
in the plasma-sprayed coatings reduces the mechanical
strength and load bearing capacity compared to the hybrid-
LVOF-sprayed coatings.
The SEM micrographs of Vickers indentation for frac-
ture toughness calculation are shown in Fig. 6. The crack
J Therm Spray Tech

Fig. 7 Residual stress measurement graphs, for plasma-sprayed coatings: (a) intensity vs. 2h (b) d-spacing vs. Sin2(Psi) and; for hybrid-LVOF
coatings: (c) intensity vs. 2h (d) d-spacing vs. Sin2(Psi)

generation at the indentation diagonal with a progression approximate the same for both coatings, but the length of
parallel to the coating–substrate interface can be observed cracks was different revealing the difference in coating
for both coatings. The indentation diagonal’s lengths were fracture toughness, the hybrid-LVOF-sprayed coating

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Fig. 7 continued

exhibiting a higher fracture toughness. The fracture The better fracture toughness of the hybrid-LVOF-
toughness values calculated by Eq 1 are 0.91 ± 0.38 and sprayed Al2O3 coating was due to a denser microstructure
1.1 ± 0.29 MPaHm for plasma and hybrid-LVOF-sprayed with a lower porosity. The high degree of splat deformation
coatings, respectively. and good inter-splat bonding could be another possible

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reason for higher fracture toughness in the hybrid-LVOF
coatings.
The measurement of fracture toughness from the coating
cross section tells us about the splat cohesion strength in
coatings. In the hybrid-LVOF process, the high particle
impact velocity promotes the level of compressive stress in
the coating due to impact-induced penning effect on the
previously deposited coating layers. This could result into
an increase in the fracture toughness of the coating. The
residual stress values were found to be 494.6 ± 93.8 and
- 171.7 ± 103.1 MPa for the plasma and hybrid-LVOF-
sprayed coatings, respectively. The stress intensity versus
the 2h peak position is shown in Fig. 7a and c for the
plasma and hybrid-LVOF-sprayed coatings, respectively.
In Fig. 7d, a decrease in the d-spacing value with Sin2(Psi)
shows the compressive nature of the residual stress in
hybrid-LVOF coating, while plasma-sprayed coating
showed opposite trend i.e. tensile residual stresses
(Fig. 7b).
Surface Roughness and Adhesion Bond Strength
High surface roughness of thermally-sprayed coatings is
undesirable as it leads to damage of coating under service.
Generally, they need to be finished in order to achieve an
acceptable surface roughness. However, ceramic-based
coatings are difficult to machine due to their lower fracture
toughness and fragile nature of coating. In this study, the
average surface roughness of the as-sprayed plasma and
hybrid-LVOF alumina coatings was 7.5 ± 1.2 and
2.9 ± 0.5 lm, respectively, as shown in Fig. 3. The lower
Ra of the hybrid-LVOF-sprayed coatings is an advantage in
comparison with plasma-sprayed coatings i.e the coating
can be used directly without any post processing, viz.
machining and grinding. Polishing of hybrid-LVOF-
sprayed coating results in super finishing.
The obtained average adhesion strength value of
plasma-sprayed and hybrid-LVOF-sprayed Al2O3 coating
was found to be 52.95 ± 5.27 and 61.23 ± 4.57 MPa,
respectively. The hybrid-LVOF-sprayed coatings have less
interfacial porosity than plasma-sprayed coatings, which
could result in a better cohesion strength. During the test,
that plasma-sprayed coating failed from the coating–sub-
strate interface (adhesive failure), while the hybrid-LVOF-
sprayed coating showed a combination of adhesive and
cohesive failure. It was also noted that only a small area
failed adhesively, which reflects the higher bond strength
of hybrid-LVOF-sprayed coating.
Dielectric Strength of the As-sprayed Coatings
The dielectric strength of coating (kV/mm) can be mea-
sured as the ratio of breakdown voltage to coating
thickness. Plasma-sprayed Al2O3 coatings generally have a
dielectric strength in the range of 10-30 kV/mm (Ref
21, 23). Their dielectric strength decreases with increasing
porosity, cracks and other defects (Ref 21). Structural
changes due to phase transformation during spraying can
also significantly affect the dielectric strength of coating. In
this work, the dielectric strength of hybrid-LVOF and
plasma-sprayed Al2O3 coating was 15.4 ± 0.7 and
11.8 ± 0.9 kV/mm, respectively. The lower porosity in
hybrid-LVOF-sprayed coating could be a reason for a
higher dielectric strength. The content of a-Al2O3 phase
was also reported to be beneficial for dielectric strength, as
the c-Al2O3 phase is more susceptible to absorb water,
which affects the dielectric properties (Ref 24).
Conclusions
Al2O3 coatings were deposited on steel substrate by plasma
and hybrid-LVOF spraying and were investigated with
respect to microstructural changes, mechanical properties,
bond strength and phase transformation. The following
conclusions can be drawn from this study. The coatings
deposited by the newly developed hybrid-LVOF spray
process exhibit better structural and mechanical properties
than plasma-sprayed coating. A higher particle velocity in
hybrid-LVOF spraying resulted in sufficient plastic defor-
mation of molten and semi-molten Al2O3 particles and led
to lower porosity and higher bond strength. A significant
retention of a-Al2O3 phase (47.9%) in the as-sprayed
hybrid-LVOF coatings is beneficial in improvement of
mechanical properties as compared to plasma spraying
(7.5%). The new process of coating has also less health
hazards than plasma spray as the radiation and noise level
are much lower. This newly developed thermal spray
process could be an alternative to conventional plasma
spraying technology.
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