j o u r n a l o f m a t e r i a l s p r o c e s s i n g t e c h n o l o g y 2 0 4 ( 2 0 0 8 ) 221–230

journal homepage: www.elsevier.com/locate/jmatprotec

Microstructural, thermal and mechanical properties

of HVOF sprayed Ni–Al-based bond coatings
on stainless steel substrate

O. Culha a , E. Celik a , N.F. Ak Azem a , I. Birlik a , M. Toparli a,∗ , A. Turk b

a Dokuz Eylul University, Engineering Faculty, Department of Metallurgical
and Materials Engineering, Buca 35160, Izmir, Turkey
b Sakarya University, Engineering Faculty, Department of Metallurgical

and Materials Engineering, 54187 Sakarya, Turkey

a r t i c l e i n f o a b s t r a c t

Article history: This work focuses on the microstructural, thermal and mechanical properties of NiAl coat-
Received 16 March 2007 ings fabricated on 316 L stainless steel substrates by using the high-velocity oxygen fuel
Received in revised form (HVOF) method. With this regard, NiAl-based coatings were fabricated on 316 L stainless
10 October 2007 steel substrates by using HVOF technique. The produced coatings were extensively ana-
Accepted 5 November 2007 lyzed with respect to X-ray diffraction (XRD), optical microscope (OM), image analyzer,
scanning electron microscope (SEM), microhardness and surface roughness testers. Adhe-
sion strength of the coatings was also measured by using a scratch tester. The effect of
Keywords: thermal cycling on the failure behaviour of the Ni–Al-based coating has been carried out
NiAl without an external load at temperatures between 47 ◦ C and 600 ◦ C for the period of 303 s
HVOF cycles. XRD study revealed that Ni3 Al phase is present in the coatings. The metallographic
Microstructure observations showed that all coatings had a similar coating microstructure and consisted
Adhesion of high-quality contact to the substrate, highly dense structure, low oxide and porosity
Thermal contents. In addition to microstructural results, microhardness values of Ni–Al-based coat-
Surface roughness ings and stainless steel were measured to be 450 HV and 220 HV before thermal cycling.
Friction These microhardness values drastically decreased after thermal cyclic tests. The adhesion
Wear strength value of Ni–Al-based coating was found that 85.3 MPa. In order to determine wear
Indentation loss, friction coefficient and wear mechanism, wear tests were performed the Ni–Al-coated
stainless steel substrates at 49 N and 89 N under dry sliding conditions through a pin-on-
plate arrangement against AISI 303 L steel counter body. Regarding as wear mechanism of
the coatings, the microstructural analysis of worn surfaces was examined by SEM. It was
found that the friction coefficients of NiAl coating for 49 N and 89 N loads were in the range
of 0.289 and 0.329 and the extent of the plastic deformation at 49 N was less than that at
89 N under dry sliding conditions. Mechanical properties of coating were examined by Shi-
madzu Dynamic Ultra-microhardness test machine for estimating Young’s modulus due to
load–unload sensing analysis and in addition to mechanical investigation of hardness–depth
curves of Ni–Al-based coatings was obtained.
© 2007 Elsevier B.V. All rights reserved.

∗
Corresponding author. Tel.: +90 232 412 7463; fax: +90 232 412 74 52.
E-mail address: mustafa.toparli@deu.edu.tr (M. Toparli).
0924-0136/$ – see front matter © 2007 Elsevier B.V. All rights reserved.
doi:10.1016/j.jmatprotec.2007.11.036
222 j o u r n a l o f m a t e r i a l s p r o c e s s i n g t e c h n o l o g y 2 0 4 ( 2 0 0 8 ) 221–230
1. Introduction
High-velocity oxygen fuel (HVOF) thermal spraying tech-
nique is used to improve roller cylinders in fabrication of
a copper wire with high purity (Nieminen et al., 1997).
In this application, steel-based roller cylinder used in the
temperature range of 600–800 ◦ C is not regularly working
during a wire-drawing process inasmuch as they are sub-
jected to wear, high-temperature oxidation and thermal
fatigue. For this application, thermally sprayed coatings
are used to improve the resistance of roller cylinders to
oxidation and surface wear and to increase their heat resis-
tance (Stewart et al., 1999). The most promising process is
HVOF technique for the deposition of the steel-based roller
cylinders as it offers an effective and economic method
of conferring wear resistance without compromising other
attributes of the component. In addition, HVOF is a ver-
satile method which can be used to deposit powders of
intermetallic compounds as dense, adherent and homoge-
neous coatings with low porosity and oxide content. These
coatings can protect the surface of critical components
used in high temperature corrosive environments (Hearley
et al., 2000). Generally speaking, WC-based powders are
deposited on the steel-based substrate by using HVOF tech-
nique (Sobolev et al., 1996; Zhao et al., 2004; Nakajima
et al., 2000; Celik et al., 2006). Sometimes, the adhesion
problems are encountered in WC-based coatings because
of high-temperature oxidation and wear interfaces between
the WC-based coating and substrate. In order to eliminate
these kinds of limitations, intermetallic bond coating such
as nickel aluminide (Ni–Al) is used in this application. To
develop thermal and mechanical characteristics of WC-based
coatings, such as high temperature corrosive resistance, oxi-
dation, friction-wear strength and mechanical integration,
Ni–Al intermetallic powder was applied by HVOF technique,
between working surface of WC-based coating and substrate
316 L stainless steel. Ni–Al-based intermetallic compounds
show excellent resistance in high temperature corrosive envi-
ronments due to the formation of a continuous, compact and
fully adherent alumina (Al2 O3 ) scale (Hearley et al., 2000).
Intermetallic Ni–Al-based compounds is a very promising
high-temperature material owing to its high melting point
(1911 K), low density (5890 kg m−3 ), high thermal conductiv-
ity (76 Wm−1 K−1 ) and excellent corrosion resistance at high
temperatures. These features permit to use Ni–Al as a coating
for high-temperature applications (Sauthoff, 1995; Ding et al.,
1997).
In HVOF thermal spraying, a gaseous or liquid fuel is pre-
mixed with oxygen at high pressure and flow rates, before
entering an internal combustion chamber. The oxy-fuel mix-
ture is continuously ignited and the combustion products
accelerated along the gun barrel nozzle to produce a super-
sonic flame (∼2000 m s−1 ). Altering the gas flows and mixing
ratios, the ratio of fuel to oxygen will influence both the flame’s
temperature and velocity. This will ultimately affect the power
output P (kW) of the HVOF gun, which can be expressed
as
P = Hc
where v is the flow rate of fuel (l s−1 ),  is the stoichiometric
ratio of fuel to oxygen and Hc is the heat of combustion of the
fuel. Propylene was used throughout as the fuel gas (Hearley
et al., 2000; Sierra and Vázquez, 2005, 2006).
In this study, we draw attention to microstructural, ther-
mal and mechanical properties of Ni–Al-based bond coatings
between WC-based coating and stainless steel substrates
by HVOF process for the roller cylinder. In this context,
Ni–Al-based coatings were fabricated on 316 L stainless steel
substrates by using HVOF technique. The produced coatings
were characterized by X-ray diffraction (XRD), optical micro-
scope, image analyzer, scanning electron microscope (SEM),
microhardness and surface roughness machines. Adhesion
properties were investigated by using the scratch tester. Ther-
mal cycling tests of the Ni–Al-based coating has been carried
out without an external load in the temperature range of
47–600 ◦ C and for the period of 303 s. Wear behaviour of NiAl
coatings was investigated using the friction and wear tester.
The worn surfaces were examined by means of SEM. Mechani-
cal properties (hardness and Young’s modulus) of Ni–Al-based
bond coatings were obtained from micro-indentation test.
2. Theoretical background of indentation
properties
Dynamical hardness and load–penetration depth measure-
ments of Ni–Al-based coating were obtained in order to
determine modulus and hardness values under different
applied peak load. The three key parameters needed to deter-
mine the hardness and modulus are the peak load (Pmax ), the
contact area (Ac ) and the initial unloading contact stiffness (S).
Similar to the conventional microhardness testing, the micro-
indentation hardness is usually defined as the ratio of the
peak indentation load, Pmax (mN), to the projected area of the
hardness impression, Ac (␮m2 ), i.e. (Uzun et al., 2005).
Pmax Pmax
H= = (Ac = 26.43h2c ) (2)
Ac 26.43h2c
Different approaches for deducing the contact depth, hc , from
the resultant load–displacement curve have been purposed
and perhaps the most widely used one is that of Oliver and
Pharr (1992). The Oliver and Pharr data analysis procedure
begins by fitting unloading curve to an empirical power-law
relation.
m
P = ˛(h − hf ) (3)
where P is the indentation load, h is the penetration depth,
hf is the final unloading depth and ˛ and m are empirically
determined fitting parameters. Using the initial part of the
unloading curve, both stiffness and contact depth are deter-
mined by differentiating Eq. (3) at the maximum depth of
penetration, h = hmax . Then, the stiffness of the contact is given
by
dP 2 
S= = √ Er Ac (4)
(1) dh 
 j o u r n a l o f m a t e r i a l s p r o c e s s i n g t e c h n o l o g y 2 0 4 ( 2 0 0 8 ) 221–230
where Er (GPa) is the reduced elastic modulus (Uzun et al.,
2005).
In this study, the Oliver and Pharr method was used to cal-
culate the initial stiffness (S), contact depth (hc ) and hence
reduced modulus (Er ) and hardness (HV).
1 1 − 2 1 − 02
= +
Er E E0
where E (GPa) and  are Young’s modulus and Poisson’s ratio
for the specimen, and E0 and 0 are the same parameter for the
indenter (De Fazio et al., 2001). The development of indenta-
tion methodologies for the micromechanical characterization
of materials requires a precise understanding of the correla-
tion between uniaxial mechanical properties and hardness.
One of such fundamental correlations was found by Tabor for
pyramidal (Vickers) indenters (Tabor, 1951). Tabor proposed
that hardness is, to a great extent, proportional to the uniaxial
stress at a plastic strain of 0.08. That is to say,
H = Cr
where H (GPa) is the Vickers hardness of the material, C = 3.3,
and  r is the uniaxial stress corresponding to a characteristic
uniaxial strain (εr ) of 0.08 (Tabor, 1951).
3. Experimental procedure
A Metco Diamond Jet (DJ) 2600 HVOF spray system was used
to deposit Ni–Al-based metallic powders. The powder to be
sprayed was injected either axially or radially, depending on
gun design, into the flame under pressure using an inert gas.
Once in the flame the powder is rapidly and uniformly heated
up to, or close to its melting temperature and accelerated along
the gun barrel nozzle towards the substrate, reaching typical
velocities of 600–1000 m s−1 . On impinging the substrate, the
molten powder particles deform, spread laterally and rapidly
solidify to form many overlapping and connected lenticular
‘splats’ or lamella. This microstructure is typical of ther-
mally sprayed coatings. The higher particle velocities achieved
with HVOF spraying lead to less oxidation or volatilizations
with improved coating adhesion and lower porosity, when
compared to other spraying processes such as plasma spray
method (Sierra and Vázquez, 2005, 2006). There are numerous
optical techniques available, including the optical micro-
scope (OM), scanning electron microscope (SEM) and X-ray
diffraction (XRD). The full coating microstructure description
contains such information as; chemical composition (at the
macro- and microstructure scale), grain morphology and its
orientation, defects (such as voids or second phases) and
coating thicknesses. Mechanical properties such as micro-
hardness, tensile strength, fracture strength, elastic modulus,
toughness, porosity and wear resistance can all be identified
using mechanical testing equipments.
3.1. Production and characterization of coating
The 316 L stainless steel with 0.030% C, 1% Si, 2% Mn, 0.045%
P, 0.030% S, 16–18% Cr, 2–3% Mo and 10–14% Ni composition
223
Table 1 – Spray parameters employed during HVOF
spraying
Parameters Values
−1
Oxygen flow rate (l min ) 130
Fuel gas (hydrogen) flow rate (l min−1 ) 400
Carrier gas (nitrogen) flow rate (l min−1 ) 18
(5) Spray distance (mm) 250
Substrate velocity (horizontal plane) (m s−1 ) 1
Gun traverse speed (vertical plane) (mm s−1 ) 5
Number of passes 20–30
was used as a substrate because of its industrial applications
of rolling, wire-drawing, high temperature moulding com-
ponent and extrusion. The substrates having dimension of
50 mm × 25 mm × 2 mm were grit-blasted on one side to clean
and roughen the surface. This process was performed for
a period of ∼30 s with 35 grit alumina powders using com-
pressed air at a pressure of ∼400 kPa. One type Ni–Al-based
feedstock powders were used in this work, namely conven-
(6) tional sintered and crushed powders. Ni–Al-based feedstock
powder was used in this work, namely conventional sintered
and crushed powders with grain size of approximately 11 ␮m.
Powder consist of 95% Ni and 5% Al (Celik et al., 2006; METKO,
2001). A Metco Diamond Jet (DJ) 2600 HVOF spray system was
used to deposit coating from Ni–Al-based metallic powders
using the spray parameters listed in Table 1. The ratio of
oxygen:hydrogen flow rate was chosen to be approximately
75% of stoichiometric. The substrates were placed on to a
turntable and rotated to give an effective horizontal traverse
rate of 1 m s−1 whilst the gun traversed vertically at a rate
of 0.005 m s−1 . The powder carrier gas was nitrogen and the
substrates were cooled with compressed air jets during and
after spraying. Further details as for deposition of the coat-
ings can be found in (Celik et al., 2006; METKO, 2001; Ak et al.,
2003). In order to verify crystallinity of the coatings, XRD of as-
sprayed coatings was performed on a Rigaku D/Max. 2200/RC
Model diffractometer with Cu K␣ radiation (1.5406 Å) using a
0.05◦ step size and a 2 s dwell time. Prior to microstructural
observations, cross-sections of the coatings were obtained
by embedding in cold mounting resin followed by grinding
and polishing, then sputter-coating with gold. Coating cross-
sections were cut from the bulk using a spark wire cutter.
An optical microscope was used to examine cross-sectional
area of the coatings. The coating thickness was measured
by the optical microscope. The porosity of layers was mea-
sured using an image analyzer (LUCIA 4.21). At least 10 fields
were measured at 200× magnification and the porosity val-
ues were averaged, as mentioned in experimental results. The
coating structures were examined using a JEOL JJM 6060 scan-
ning electron microscope (SEM). Microhardness tests were
performed using a Carl Zeis microhardness tester with a 80 g
load and a dwell time of 15 s. Hardness quoted are an aver-
age of five indents (with the quoted range being the standard
error in the mean) which were placed in the middle of the coat-
ings on cross-sectioned and polished samples parallel to the
coating/substrate interface. Surface roughness measurements
were carried out by using Mitutoyo SJ-301 Surface Roughness
Tester. Adhesion strength of the coatings was measured by
using Shimadzu Scanning Scratch Tester SST-W101. In this
224 j o u r n a l o f m a t e r i a l s p r o c e s s i n g t e c h n o l o g y 2 0 4 ( 2 0 0 8 ) 221–230
technique, the load on a Rockwell C diamond with tip radius of
stylus (R) of 15 ␮m was linearly increased from 0 mN to 98 mN
at loading speed of 1 ␮m s−1 and scratch speed of 2 ␮m s−1 as
the diamond is drawn across the coating surface. The test-
ing temperature and humidity percentage are 20.3 ◦ C and 50%,
respectively. After microhardness value of metal substrate was
converted to Brinell hardness (H) from Vickers microhardness
by using Standard Hardness Conversion Tables for Metal (Celik
et al., 2006; Callister, 1997), the adhesion strength (F) of the
coatings was calculated as MPa unit by using Eq. (7) for average
value of three measurements. The scratch was examined with
an optical microscope and critical load (average Wc : 13 mN) at
which the coating is removed was determined. The adhesion
strength (F (MPa)) was calculated by using Eq. (7):
H Te 88 Multi-station Friction and Wear Test Machine. The loads
F= 1/2
(7)
[(R2 H − Wc )/Wc ]
where H is the Brinell hardness value in kg mm−2 of the 316 L
stainless steel substrate and R is the radius of stylus in ␮m.
As the test force applied to coating increases, peeling of coat-
ing occurs. At this time peeled pieces of coating cause a high
frequency noise in a cartridge output signal. Detecting this
noise makes it possible to determine a critical force. Normally,
this critical force can be used the adhesion value of coat-
ing. However, in the case that a hardness of the substrate
has been known, Eq. (7) can show adhesion strength. As a
result of this, test force–cartridge output graph is obtained
from this measurement. Cartridge output (%) represents per-
centage of indentation of the stylus as a function of loading
during the test. The percentage increases with an increasing
load, that applied by stylus, due to the adhesion resistance of
the coating to substrate (Celik et al., 2006; Shimadzu, 2003).
The adhesion strength of the impinging particle to the sub-
strate is dependent on mechanical, metallurgical–chemical
and physical mechanisms. Subsequently, diffusion or alloy-
ing may occur by forming intermetallic compounds and this
is known as the metallurgical–chemical adhesion mechanism.
The physical bonding is a result of particle adhesion to the
substrate by Van Der Waals forces (Celik et al., 2006; METKO,
2001). Cohesive strength depends on the roughness, tempera-
ture difference and bond/cohesive strength of the previously
coated surface (Shimadzu, 2003; Ak et al., 2004; Kusoglu et
al., 2005; Celik et al., 2003; Cetinel et al., 2003; Uyulgan et al.,
2003; Scrivani et al., 2001; Liao et al., 2000). The bond strength
achieved by the HVOF system is 25% greater than that found
using other thermal spraying processes. This is achieved due
to the high velocities of the coating particles that are exposed
during flight, causing the particles to forge or weld together
on impact with previously deposited material. The adhesion
strength of HVOF sprayed layers also depends on the hard-
ness of impinged particles which is dominant of the anchoring
effect on the substrate surface and the kinetic energy of the
particle (Nieminen et al., 1997; Callister, 1997; Tekmen et al.,
2004).
3.2. Thermo-mechanical property
The effect of thermal cycling on the failure behaviour of the
Ni–Al-based bond coating has been carried out without an
external load. A special designed furnace has been used for
the thermal cycling tests. In order to verify the thermal cycling
tests, at least three samples have been used. The samples were
heated in an electrical resistance movable furnace and cooled
by a forced air current. During the thermal cycling test, a ther-
mocouple has been used to measure the temperature of the
sample. The temperature range was kept between 47 ◦ C and
600 ◦ C and the period for each cycle was 303 s.
3.3. Friction and wear properties
Wear tests of NiAl bond coating deposited on stainless steel
substrates were performed at 49 N and 89 N under dry slid-
ing conditions through a pin-on-plate test mode against AISI
303 L steel counter body with a diameter of 5 mm using Plint
were applied to the sliding sample via a stationary pin. Sam-
ple was mounted on a plate that has a reciprocating motion
with 1 Hz and 12 mm stroke while pin was fixed. The total slid-
ing distance was 9.6 m. Further details regarding wear tests
of coatings were described elsewhere (Celik et al., 2003, 2006;
METKO, 2001; Kusoglu et al., 2005; Cetinel et al., 2003; Uyulgan
et al., 2003; Scrivani et al., 2001). The microstructural analysis
of the worn surfaces was examined by SEM.
3.4. Ultra-microhardness study of coating
Mechanical and elastic properties (hardness and Young’s
modulus) of Ni–Al-based coating were obtained from
load–indentation curves by using ultra-microhardness tester
under 300 mN, 350 mN, 400 mN and 450 mN applied peak load.
The qualities of small size and non-destructive test capabil-
ity make the indentation technique superior to the tension
test. For very small volumes of material, the uniaxial test is
inapplicable. Furthermore, the structural materials may not
be removed to do the tension test in most cases, for instance,
the materials used for coatings (Yao, 2005).
4. Results and discussion
4.1. Characterization and thermo-mechanical
experiment
Fig. 1 shows XRD pattern of Ni–Al-based bond coating
deposited on stainless steel substrate by HVOF technique. In
the XRD pattern of the coating, peaks indexed to Ni3 Al cor-
responding to (1 1 2) orientation. This result is a fine point
Fig. 1 – XRD pattern of NiAl coating deposited on stainless
steel substrate by HVOF technique.
 j o u r n a l o f m a t e r i a l s p r o c e s s i n g t e c h n o l o g y 2 0 4 ( 2 0 0 8 ) 221–230
in this work due to the fact that Ni3 Al has received strong
interest as a high-temperature material because of its anoma-
lous strengthening with increasing temperature as indicated
(Scrivani et al., 2001; Liao et al., 2000; Tekmen et al., 2004; Yao,
2005; Dent et al., 2002; Hearley et al., 1999).
Microstructural properties of the coatings on stainless steel
substrate were examined as a combination of optical micro-
scope, image analyzer and SEM. In HVOF system, the particle is
initially melted and propelled out from the gun in the form of a
sphere then, at its first contact with the substrate, the impact
creates a shock wave inside the lamella and in the substrate.
Post-impact the particle forms into a pancake shape. In addi-
tion, the coating microstructure is influenced by not only both
particle velocity and its temperature but also spray distance.
Notably, their effects make lamella or flower type microstruc-
tures (Celik et al., 2006; Ak et al., 2004; Dent et al., 2002). The
solid particles may rebound or remain weakly connected to
the rest of the coating, reducing its strength (Hearley et al.,
2000; Celik et al., 2006; Ak et al., 2004; Dent et al., 2002). That
is why careful optimization of spray parameters is necessary
to eliminate such problems. As shown in Fig. 2a and b, SEM
micrograph of the coating cross-sections revealed excellent
homogeneity and uniformity. In our study, it can clearly be
seen from Fig. 2a and b that the coating is dense compar-
ing other thermal spray techniques (METKO, 2001) and has
very low oxide content and high-quality contact with the sub-
strate, indicating a superior bonding to the substrate. The
Fig. 2 – A cross-sectional SEM micrograph of NiAl coating
on stainless steel sample.
225
Fig. 3 – Critical force values of NiAl coating deposited on
stainless steel substrate.
Ni–Al-based particles distribute uniformly in the coating. The
metallographic analysis of the coatings shows 2.5% porosity.
Compared to the previous studies (Celik et al., 2006), porosity
values of HVOF sprayed Ni–Al-based coating can be accept-
able. Porosity in the coating microstructure is an important
issue in thermal spraying technique as it is owing to this phys-
ical property that many coating mechanical properties such as
Young’s modulus and adhesion strength differ from those of
counter body bulk materials. Compared to the other spraying
techniques such as electric arc, flame, plasma spraying, deto-
nation gun and/or their different configurations, HVOF process
exhibits the lowest porosity of all known thermal spraying
methods (METKO, 2001), as the high impact velocity, com-
presses most air pockets out of microstructure (Nieminen et
al., 1997). In addition to the microstructural examination, the
thickness of Ni–Al layer was measured to be 595 ␮m.
One of the main issues in the coating characterization is
the adhesion of coating to the substrate. Owing to this rea-
son, the investigation of adhesion of Ni–Al-based coatings
on stainless steel substrate is based on optical microscope
and SEM observations of the surface of scratches, and on
the analysis of scratch tester that allows the scratch criti-
cal load values to be determined. These critical normal load
values correspond to be the first peak in the cartridge-test
force graphical curve obtained from scratch tester machine.
Figs. 3 and 4 show critical force values and scratch image of
Ni–Al-based coating on stainless steel substrate, respectively.
In the case of the Ni–Al-based coatings, the first failure of
the coating by cracking and spallation on either side of the
scratch was detected in the critical load range of 6–26 mN.
The adhesion strength value of Ni–Al coatings was calcu-
lated as 85.3 MPa using Eq. (7). Adhesion strength values of
carbide compounds such as WC-based and CrC-based coat-
ings are between 80 MPa and 90 MPa, on the other hand
adhesion strength value of nickel-, chromium-, molybdenum-
based super alloys and cobalt-based alloys is approximately
65 MPa (Celik et al., 2006; METKO, 2001). As a consequence
adhesive strength of coating was increased by carbide com-
pounds because of their hardness effect. According to Eq. (7),
the average adhesion strength value of Ni–Al-based coating
was found to be 85.3 MPa (average of three measurements)
and its standard deviation was 15 MPa. Therefore the result
is clearly acceptable for rolling process application.
226 j o u r n a l o f m a t e r i a l s p r o c e s s i n g t e c h n o l o g y 2 0 4 ( 2 0 0 8 ) 221–230
Fig. 4 – SEM images of scratched NiAl coating on stainless
steel sample.
Fig. 5 – Microhardness values of NiAl coating deposited on
stainless steel substrate before and after thermal cyclic.
Microhardness of the coatings was scrutinized as a func-
tion of distance from coating surface. Depending on this,
microhardness value of the coating from surface to substrate
was given in Fig. 5. As can be clearly seen from Fig. 5, micro-
hardness values of Ni–Al-based coating and stainless steel
were measured to be 450 HV and 220 HV before thermal cycling
tests, respectively. We have a good agreement with (Hearley
et al., 1999; Wang et al., 2003; Wang and Chen, 2004). Notably,
the microhardness value of the Ni–Al-based coating decreased
Fig. 6 – Surface roughness vs. wear distance for NiAl
coatings on stainless steel substrate.
Fig. 7 – (a) Friction coefficient vs. wear time curves of the
NiAl coating and mild steel substrate. (b) Wear loss vs. wear
time curves of the NiAl coating and mild steel substrate.
from 450 HV to 330 HV as a function of distance from the coat-
ing surface to substrate. The hardness values of Ni–Al-based
coating after thermal cycling tests decreased from 450–330 HV
to 320–230 HV. Because the number of cycling is a significant
parameter, microhardness values of the coatings considerably
decreased depending on increasing the number of thermal
cycling.
4.2. Friction and wear test results
The quality of surface roughness is an important requirement
for coated parts. Fig. 6 denotes surface roughness versus wear
distance for Ni–Al-based coatings on stainless steel substrate
after wear tests. The surface roughness value of as-sprayed
Ni–Al coating was measured as 8.75. Nonetheless, it can be
pointed out that when the applied load was increased in the
wear tests, surface roughness values decreased according to
Fig. 6. When the applied load was increased for wear test,
plastic deformation degree of coating under applied load was
increased. Asperities which were located at the contact region
of pin and coating were plastically deformed depending on
load variation. In addition to this, wear mechanism can be
effected by hard asperities which can be break off from surface
of coating (three-body wear mechanism). Another parameter
is wear distance which influences surface roughness. In this
 j o u r n a l o f m a t e r i a l s p r o c e s s i n g t e c h n o l o g y 2 0 4 ( 2 0 0 8 ) 221–230 227

deformation as demonstrated elsewhere (Celik et al., 2006; De

Table 2 – Friction coefficient values of stainless steel
substrate and NiAl coating
Parameters Loads (N) s
Substrate 49 0.554
NiAl coating 49 0.289
89 0.329
case, surface roughness decreases as a function of wear dis-
tance. The coefficient of the friction versus total sliding time
curve for the Ni–Al-based coating against stainless steel pin
is given in Fig. 7a, which indicates two friction regimes. At
the beginning, the friction coefficient increases till it reaches
a maximum value (s : statically friction force). The maximum
value is followed by a gradual decrease to a lower steady-state
value (d : dynamically friction force). These values of Ni–Al-
based coating and substrates that are dependent on loads are
presented in Table 2. The friction between sliding surfaces is
due to the combined effects of adhesion between flat surfaces,
ploughing by wear particles and hard asperities and asperity
Fazio et al., 2001). The static friction coefficients of the Ni–Al-
based coating and substrate for 49 N load were found to be
d
0.554 and 0.289, respectively. Furthermore, the dynamic fric-
0.417 tion coefficients of the coating and substrate were 0.417 and
0.107 0.107, respectively. In addition to these results, upon increas-
0.295
ing the applied load from 49 N to 89 N, the variation of the
static and dynamic friction coefficient concerning the coating
increased to be 0.329 and 0.295, respectively. The Ni–Al-based
coating shows better wear resistance than substrate. The vol-
ume loss versus sliding time curve for the Ni–Al-based coating
and the stainless steel substrate is denoted in Fig. 7b. When
the wear loss values of the substrate and coating were com-
pared as seen in Fig. 7b, it can be seen that the stainless steel
substrate has higher wear loss than coating at the 49 N applied
load. Although the load was increased from 49 N to 89 N, wear
loss of the coatings increased as expected, but according to
Fig. 7b it was less than substrate. The wear rate is generally
slow, but steady and continuous. As a normal load is applied,
local pressure at the asperities became extremely high. Often
yield stress exceeded, and asperities plastically deform until

Fig. 8 – Surface images of unworn and worn substrate and NiAl coating tested under 49 N and 89 N loads. The figures in (a)
and (b) represent unworn and worn substrate samples under 49 N load, respectively. The figures in (c) and (d) represent
unworn and worn NiAl coating samples under 49 N load, respectively. The figures in (e) and (f) show unworn and worn NiAl
coating samples under 89 N load, respectively.
228 j o u r n a l o f m a t e r i a l s p r o c e s s i n g t e c h n o l o g y 2 0 4 ( 2 0 0 8 ) 221–230

the real area of contact has sufficiently increased to support
the applied load (see Fig. 8b, d and f). SEM micrographs of
the wear track for the Ni–Al-based coating and the stainless
steel are depicted in Fig. 8. In addition, detailed observation of
worn samples tested under dry conditions can be character-
ized by local plastic deformations such as wear tracks, grooves,
scratches and adhesive junctions (Ak et al., 2004). The plastic
deformation of each worn and unworn samples at 49 N load
was less than that at 89 N under dry condition. The worn sur-
face of the Ni–Al coating exhibits smoother surface compare
to the unworn coating surface because of the friction and wear
mechanism.
4.3. Mechanical properties investigation
Surface roughness value of samples is an important parameter
for micro-indentation test with Dynamic Ultra MicroHard-
ness Tester. After HVOF thermal spray process, Ni–Al coating
surface roughness can be high for micro-indentation test.
So, surface polishing process is applied to cross-sectional
part of Ni–Al coating for decreasing roughness. Because of
micro-indentation test result’s sensitivity and homogeneity,
polishing process must be applied whole cross-sectional sur-
face to minimize Ra value of samples. After polishing process,
roughness of cross-sectional part of Ni–Al-based coatings
decrease from 5.2 ␮m to 0.15 ␮m.
The mechanical properties such as hardness, Young’s mod-
ulus, ductility, etc. are important parameters for Ni–Al-based
bond coatings between WC-Co surface coatings and stain-
less steel substrate. Shimadzu Dynamic Ultra-MicroHardness
Testing machine is used for determination hardness vari-
ation and Young’s modulus of Ni–Al-based bond coatings.
Different load range such as 450 mN, 400 mN, 350 mN and
300 mN is applied for determination of hardness and Young’s
modulus. Indentation experiments of Ni–Al-based coating
showed that when applied peak load is increased from 300 mN
to 450 mN, hardness of coating decreases from 745 DHV
(Dynamic Hardness Vickers) to 515 DHV. Dynamic Hardness

Fig. 9 – (a) Hardness determination of NiAl-based bond coatings under 300 mN, 350 mN, 400 mN and 450 mN applied peak
load and (b) elastic modulus investigation of NiAl bond coatings under 300 mN, 350 mN, 400 mN and 450 mN by load–unload
test mode of indentation.
 j o u r n a l o f m a t e r i a l s p r o c e s s i n g t e c h n o l o g y 2 0 4 ( 2 0 0 8 ) 221–230 229

Table 3 – Indentation experiments of Ni–Al-based bond coating under 300 mN, 350 mN, 400 mN and 450 mN peak load
Material Indentation Maximum depth (␮m) Residual depth (␮m) Hardness (DHV) Calculated Young’s
load (mN) modulus (GPa)

450 2.61 2.22 515 112

Ni–Al-based 400 2.25 1.91 605 116
bond coating 350 2.05 1.77 695 118
300 1.71 1.42 745 139

Table 4 – Hardness and yield strength study of Ni–Al-based coating

Material Indentation hc (␮m) Calculated Amax (␮m2 ) Calculated hardness (GPa) Theoretical yield
load (mN) strength (GPa)

450 2.30 140 3.22 0.97

Ni–Al-based 400 1.98 104 3.85 1.16
bond coating 350 1.87 92 3.80 1.15
300 1.55 64 4.69 1.42

results of Ni–Al-based coatings at 450 mN, 400 mN, 350 mN and
300 mN peak loads are shown in Fig. 9a. The figures, which
were experimentally constructed using the data taken from
the loading part of indentation analysis at applied peak loads
from cross-sectional part of Ni–Al-based coating, represented
the load dependency of hardness. DHV numbers of coatings
decrease with increasing penetration depth at applied peak
loads. Hardness investigations have confirmed that DHV num-
ber of materials were indentation size dependent, especially
at lower peak loads. Increase in hardness with decreasing
applied peak load cause from differences in indentation depth,
therefore this effect is called indentation size effect (Uzun et
al., 2005).
The load–unload mode (load–displacement) curves are
shown in Fig. 9b. It is represented the 450 mN, 400 mN, 350 mN
and 300 mN applied loads as a function of the displacement
(elastic and plastic) of the indenter with respect to the initial
position of the surface.
Table 3 shows the hardness, Young’s modulus, residual
depth and maximum depth value of samples under 450 mN,
400 mN, 350 mN and 300 mN applied peak loads. The calcu-
lated Young’s modulus of Ni–Al-based coating decreases with
increasing applied peak loads. As seen in Fig. 10, the elastic
modulus of Ni–Al-based bond coating decrease from 139 GPa
to 112 GPa with increase in applied peak load from 300 mN to
450 mN (Wang and Chen, 2004).
Theoretical calculation of Ni–Al-based bond coating’s yield
strength needs indentation parameters such as hc , Amax and
applied peak load (Uzun et al., 2005; Tabor, 1951). Table 4
shows the calculated hardness and theoretical yield strength
values of Ni–Al-based bond coating under 300 mN, 350 mN,
400 mN and 450 mN applied peak loads. When applied peak
load is increased from 300 mN to 450 mN, Vickers hardness
value of Ni–Al-based bond coatings decreases from 4.69 GPa
to 3.22 GPa. Like hardness variation, theoretical yield strength
values of Ni–Al-based bond coating decrease from 1.42 GPa to
0.97 GPa by increasing in applied peak load from 300 mN to
450 mN.
5. Summary and conclusion
The present research paper has summarized the microstruc-
tural, thermal and mechanical properties of Ni–Al-based
coatings fabricated on 316 L stainless steel substrates by using
the HVOF thermal spraying method as the bond layer for the
roller cylinder. It can be concluded as follows:

(1) XRD pattern revealed that Ni–Al-based coating had Ni3 Al

phase on surface.
(2) SEM micrograph of the coating cross-sections demon-
strated excellent homogeneity and uniformity. The
coating possessed low oxide content, low porosity and
superior contact with the substrate. The thickness of
Ni–Al-based layer is 595 ␮m. In addition, un-melted or
semi-melted particles were not observed in these coatings.
(3) The first failure of the coating by cracking and spallation on
either side of the scratch was detected in the critical load
range of 6–26 mN. The adhesion strength values of Ni–Al-
based coatings were, respectively calculated as 85.3 MPa.
(4) Microhardness values of Ni–Al coating and stainless steel
were measured to be 450 HV and 220 HV before thermal
Fig. 10 – Calculated elastic modulus variation of NiAl bond cycling tests, respectively. The microhardness value of the
coating by indentation peak load. Ni–Al-based coating decreased from 450 HV to 330 HV as a
230 j o u r n a l o f m a t e r i a l s p r o c e s s i n g t e c h n o l o g y 2 0 4 ( 2 0 0 8 ) 221–230
function of distance from the coating surface to substrate
after thermal cycling.
(5) The surface roughness values of as-sprayed Ni–Al-based
bond coating was measured as 8.75 ␮m and 6 ␮m, respec-
tively. Surface roughness decreases as a function of wear
distance.
(6) The friction coefficients of Ni–Al bond coatings for 49 N
and 89 N loads were found to be 0.289 and 0.329, respec-
tively. When the applied load was increased from 49 N to
89 N, wear loss of the coatings as expected increased, but
less than substrate.
(7) Dynamic hardness determinations of Ni–Al bond coating
showed that increase in applied peak load from 300 mN
to 450 mN, hardness of coating decreases from 745 DHV to
515 DHV.
(8) The calculated Young’s modulus of Ni–Al-based coating
decreases with increasing in applied peak load. The elas-
tic modulus results showed that when applied peak load
is increased from 300 mN to 450 mN, elastic modulus
decreases from 139 GPa to 112 GPa.
Acknowledgement
The authors would like to thank Plasma Technique, Istanbul,
Turkey, for providing the coating process.
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