Journal of Materials Processing Technology 174 (2006) 204–210

Three-point bend testing of HVOF AMDRY 9954 coating

on Ti–6Al–4V alloy
D. Al-Anazi a , M.S.J. Hashmi a , B.S. Yilbas b,∗
a Dublin City University, Ireland
b KFUPM, Saudi Arabia

Received 10 August 2005; accepted 3 November 2005

Abstract
HVOF coating of AMDRY 9954 powders onto Ti–6Al–4V alloy is considered. Three-point bending tests are carried out to examine the tensile-
shear response of the coating under the bending load. The study is extended to include the heat treatment of the workpieces after the coating process
prior to three-point bending tests. The morphological and microstructural analyses are carried out using scanning electron microscopy (SEM).
Finite element method (FEM) is introduced to simulate the bending situation and predict the stress distribution in the workpieces. It is found that
coating with small porosity and voids is achieved. Elongated cracks are developed in the coating in the region of deflection of the workpiece during
the bending tests. This, in turn, results in partial attachment of the coat onto the base material without complete peeling off from the substrate
surface due to stress relaxation at coating interface. However, the coating with severe crack formation and total peeling off from the substrate
surface are also observed, which is more pronounced for heat treated workpieces.
© 2006 Elsevier B.V. All rights reserved.

Keywords: HVOF coating; Three-point bending; Microstructure; FEM

1. Introduction Considerable research studies are carried out to examine

Coating of high-temperature components is required in power
generating units for preventing the surface of the components
from excessive heating, erosion, and corrosion during the oper-
ation. Coatings applied must have resistance to high-temperature
as well as the mechanical forces. In this case, the coating mate-
rial selected for such an application must have the properties
that resistant to harsh environments as well as the coating pro-
cess must be efficient, low cost, and fast. One of the coating
methods fulfilling these conditions is High Velocity Oxy-Fuel
coating (HVOF). Although the process is fast, effective, and
low cost, due to the irregularities associated within the result-
ing coat, investigation into the process is necessary for further
improvements of coating quality. The mechanical properties
of the coating, particularly at coating-base material interface,
are important to secure the sound coating. Consequently, study
into mechanical properties of coating-base material interface
becomes essential.
∗ Corresponding author. Tel.: +966 3 860 4481; fax: +966 3 860 2949.
E-mail address: bsyilbas@kfupm.edu.sa (B.S. Yilbas).
the mechanical properties of HVOF coating. Microstructural
study of HVOF and vacuum plasma spray (VPS) MCrAlY coat-
ings were carried out by Nuutien et al. [1]. They indicated
that HVOF process resulted in improved coating microstruc-
ture with low oxide content. The behavior of nickel-based alloy
(NiCrMoAlFe) coating due to the mechanical loading was inves-
tigated by Hidalgo et al. [2]. They conducted thermal fatigue
tests and the adhesion between the substrate and the coating lay-
ers was evaluated by means of tensile tests. They showed that
the substrate-coating adherence were high and being not sig-
nificantly affected by thermal fatigue. The characterization of
HVOF coatings for petrochemical applications was carried out
by Scrivani et al. [3]. The slurry tests showed a clear discrim-
ination among the performances of various coatings. WC/Mo
compound resulted in fairly good behavior in an erosion environ-
ment and higher erosion resistance than Inconel 625 and NiAl.
A comparative study for thermal spray coating of CoNiCrAlY
bond-coat alloy was carried out by Scrivani et al. [4]. They indi-
cated that HVOF coating showed good porosity level due to high
flame velocity; however, the oxide content was high with respect
to vacuum plasma spray. Reaction-diffusion behavior of ther-
mally sprayed MCrAlY coatings on Ni-based super alloy was

0924-0136/$ – see front matter © 2006 Elsevier B.V. All rights reserved.
doi:10.1016/j.jmatprotec.2005.11.038
 D. Al-Anazi et al. / Journal of Materials Processing Technology 174 (2006) 204–210 205

Table 1
Nomenclature Process parameters of HVOF thermal spray
Oxygen pressure (kPa) 1023
B strain displacement gradient matrix Fuel pressure (kPa) 590
de elemental nodal displacement vector Air pressure (kPa) 720
di nodal displacement vector Powder feed rate (m3 /h) 0.85
D elasticity matrix Spray rate (kg/h) 6.5
E modulus of elasticity Spray distance (m) 0.31
fB applied body force vector
Fb elemental applied body force vector
fC applied concentrated force vector lifetime of coating. The analysis of the mechanical properties
Fc elemental applied concentrated force vector of aluminum and iron-based thermal spray coatings was car-
fS applied surface force vector ried out by Burkle et al. [10]. They showed that the method
Fs elemental applied surface force vector used permitted the determination of pure coating material static
Ft elemental thermal load vector and dynamic mechanical properties without substrate influence
Ke elemental stiffness matrix over a wide temperature range. The microstructural analysis of
L differential operator matrix CoNiCrAlY coatings produced by HVOF spraying was carried
N matrix of shape (or interpolation) functions out by Turner et al. [11]. They indicated that the oxide content
t time of HVOF sprayed coatings should be kept as low as possible
␦u virtual displacement vector in order to make the post-heat treatment active in producing a
δU virtual internal work dense microstructure with correct phase structure.
δV virtual external work In the present study, HVOF coating of AMDRY 9954
x distance along longitudinal direction (x-axis) (CO38 Ni21 Cr8 Al0.5 Y) powders on Ti–6Al–4V alloy is consid-
y distance along transverse direction (y-axis) ered. Mechanical properties of coating interface is examined
αe coefficient of thermal expansion through three-point bending tests. The bending test conditions
ε total strain vector are simulated using the finite element method (FEM) and stress
␧m mechanical strain vector fields in the coatings as well as across the coating-base sub-
␧t thermal strain vector strate material are predicted numerically. In order to investigate
ε equivalent strain the metallurgical changes before and after the mechanical tests,
ν Poisson’s ratio SEM is carried out. The study is extended to include post-heat
treatment; in which case, the changes in mechanical and metal-
lurgical properties in coating are investigated due to post-thermal
processing prior to bending tests.
investigated by Teratani and Harada [5]. They showed that the
coatings sprayed by atmospheric plasma spraying process con- 2. Experimental
tained larger amount of oxides than the coating by low-pressure
plasma spraying process and the diffusion of aluminum and other A hybrid HVOF coating unit was employed to spray the coating powder.
components was more inhibited in the former than the later. Propane was used in the combustor and flow was centered by using axial pow-
The effect of residual stress in HVOF carbide coatings on der feeding with auxiliary air, which surrounded the particle stream during the
spraying. The spraying properties are given in Table 1.
fatigue life in bending of thermal spray coated aluminum was AMDRY 9954 (CO38 Ni21 Cr8 Al0.5 Y) powders was used. The powder had a
studied by McGrann et al. [6]. They showed that the fatigue particle distribution between 20 and 35 ␮m with spherical morphology with
life of WC-coated specimens was directly related to the level of some small and local satellite attachments (Fig. 1). It had excellent high-
compressive residual stress in the coating. Moreover, in some temperature oxidation and corrosion properties. The base material, on which
cases, the fatigue life could be increased by a factor of 35% the powder was sprayed, was Ti–6Al–4V alloy.
The schematic view of three-point testing unit is shown in Fig. 2. A computer
increasing the compressive residual stress in the coating. The controlled INSTRON 300 instrument is used in the three-point bending tests.
influence of thermal process selection and corresponding bond- The photograph of a workpiece after the bending test is shown in Fig. 3.
coat surface roughness on thermal barrier coating performance JEOL JDX-3530 scanning electron microscope (SEM) is used to obtain
were investigated by Knight et al. [7]. They used the bond-coat photomicrographs of the cross-section and surface of the workpieces after the
deposition process and indicated that surface roughness had sig- tests.
nificant effect on the coating adhesive strength. The effects of
surface oxidation during HVOF coating process were studied by 3. Finite element modelling
Tang et al. [8]. They showed that the surface oxide that formed
on a CoNiCrAlY coating during HVOF process could signifi- To develop a finite element procedure for the stress compu-
cantly affect its subsequent mechanical behavior. The influence tation, the principle of virtual work is used. According to this
of bond-coat processes and surface characteristics on the failure principle, the equilibrium of any body under loading requires
mechanism of thermal barrier coatings was studied by Ding et al. that for any compatible small virtual displacements imposed on
[9]. They indicated that bond-coat deposition process and sur- the body in its state of equilibrium, the total virtual internal
face characteristics had significant effects on the thermal fatigue work or strain energy (δU) is equal to the total virtual external
206 D. Al-Anazi et al. / Journal of Materials Processing Technology 174 (2006) 204–210
Fig. 1. SEM micrographs of AMDRY 9954 powders used in HVOF spraying.
Fig. 2. A schematic view of three-point bending test set up.
work due to the applied thermal loads (δV), i.e. δU = δV. The vir-
tual displacements are zero at the boundary points and surfaces.
For the static analysis of problems having linear geometry and
thermo-elastic material behavior, one can derive the following
equation using the standard procedure as:



(δεT Dε − δεT Dεt )dV = ␦uT fB dV

to change at different load levels. These changes are incorporated
+ ␦uT fS dS + ␦uT fC
where V and S denote the volume and surface, fB , fS and fC
stand for the vectors of body, surface and concentrated forces,
respectively.
The elemental displacement vector de is related to the nodal
displacement vector di by:
de = N di
Fig. 3. A photograph of workpiece after the three-point bending test.
where N is the matrix of shape or interpolation functions. The
elemental strain vector ␧e is written as:
␧e = L de (11)
where L is a differential operator matrix. Consequently, the strain
vector ␧e is related to the nodal displacement vector di by:
␧e = L N di = B di (12)
where B (= LN) is the strain displacement gradient matrix. As a
result, the Eq. (10) is reduced to the following matrix form (after
the assemblage):
Kd − Ft = Fb + Fs + Fc (13)
where d is the global displacement vector and the elemental
matrices and vectors are given as:


Ke = BT DB dV = elemental stiffness matrix,


Ft = BT D␧t dV = elemental thermal load vector,


F = N T fB dV = elemental body force vector,
b


F = N T fS dS = elemental surface force vector and
s
Fc = N T fC = elemental concentrated force vector.
Eq. (13) is now expressed as:
Kd = Ft + Fb + Fs + Fc = F
where F is the global force vector. Solution of the above set
of simultaneous algebraic equations yields the unknown nodal
displacements and reaction forces. Once the displacement field
due to temperature rise in the substrate is known, then the cor-
responding strains and stresses can be calculated.
A number of material-related factors can cause the structure’s
stiffness to change during the course of an analysis. Nonlinear
stress–strain relationships of plastic causes a structure’s stiffness
(10) into an ANSYS analysis through using the appropriate element
types.
4. Results and discussions
HVOF coating of AMDRY 9954 powders on Ti–6Al–4V
alloy is considered and three-point bending tests are carried out
to investigate the coating-base material interface properties. The
(11) influence of heat treatment on interface properties are also exam-
ined. Finite element method (FEM) simulating the experimental
conditions is carried out to predict the stress field during the
bending tests.
The elastic–plastic behavior of the workpiece with coating
and without coating as well as with heat treatment is shown in
Fig. 4. The data is obtained from the three-point bend tests, which
were carried out at constant strain rate. As-received uncoated and
heat treated uncoated workpieces show similar elastic–plastic
behavior while coated workpieces differ slightly in behavior.
In this case, the plastic region for heat treated coated sample
 D. Al-Anazi et al. / Journal of Materials Processing Technology 174 (2006) 204–210
Fig. 4. Load and displacement characteristics of the workpiece after three-point
bend tests.
initiates at low load level for the same flexural displacement.
This indicates that heat treatment has an effect on the coating,
since heat treated uncoated and as-received uncoated workpieces
behave similarly, i.e., toughness of the coating changes slightly
after the heat treatment. Moreover, the abnormal behavior in the
curves are not observed. This suggests that the gradual defor-
mation of interface of the substrate material could relieve the
stress levels at the interface and this has a contributing effect on
stress relaxation. Moreover, the compressive stress generated
at the top surface of the workpiece does not generate fail-
ure, such as peeling due to elastic strain energy stored in the
coating.
Since the coated surface is placed in the bottom (opposite)
site where the three-point bend indented is applied, the coating
section of the workpiece is subjected to tensile-shear force only.
Consequently, the main failure in the coating occurs because
of the tensile-shear deformation, particularly coating-substrate
material interface. The crack in the coating is formed due to
the tensile load and initiated at the free surface of the coat-
ing as well as oxide sites in the coatings as shown in Fig. 6.
Under the tensile-shear loading, delamination above the plasti-
cally deformed region is occurred. It should be noted that during
the thermal spraying process, formation of oxidation is expect-
edly high in the free surface of the coating. This, in turn, results in
differences in stiffness in the coating. Consequently, high oxide
content in the surface region of the coating triggers early crack
Fig. 5. Coating cross-section prior and after the heat treatment process.
207
initiation and propagation along the coating and the substrate
material interface. The development of internal stress, due to
tensile-shearing force, creates local stress concentrations, partic-
ularly at defect sites in the region of coating-substrate interface.
In this case, the defect site has a significant effect on the fail-
ure mechanism. It should be noted that stress concentrations at
defect sites are, in general, higher than the mean internal stresses.
When the critical stress for crack propagation is reached in defect
sites at the interface, the entire coating fails and peels off from
the substrate material. If the crack propagation is limited to local
region, the fracture of the coating is resulted. In this case, inter-
nal stress in the coating is relaxed around the crack sites. If the
energy used to propagate the crack is dissipated, the crack can-
not extend beyond the substrate material, i.e., it terminates at the
free surface of the substrate material.
Fig. 5 shows SEM micrographs of coating prior and after the
heat treatment process. The coat cross-section reveals that the
coating consists of lamellar structure with existence of some
small voids between the splats. However, the voids are dis-
tributed randomly resulting in overall 3% porosity in the coating.
Oxidation around some splats is evident due to the oxidation
during in-flight duration of the splat before impacting the sub-
strate surface. In addition, some stringers like dark inclusions
are also observed. These are the brittle oxide particles in the
coating.
Fig. 6 shows SEM micrographs of the tensile surface as well
as the cross-section of the workpiece after the bending tests.
Multi-crack deformation in the coating is evident, which shows
that coating does not conform to the plastic deformation in
the substrate material. In some regions, crack spacing is small
indicating that the sliding and splitting deformation occurs in
the coating. However, in general, crack spacing is large and in
some regions total elimination of coating is resulted (peeling off
from the substrate surface) due to shear deformation at coating-
substrate interface. In addition, the coating fracture was brittle
and no sign of plastification was observed. The metallic particles
(splats) debond mainly through their oxide interfaces. The elon-
gated particles, particularly oxided brittle particles, promotes a
high stress concentration and crack initiation. Moreover, adhe-
sion failure was also observed resulting in separation between
the substrate and the coating. In the case of heat treated work-
pieces, thermal stresses generated along the coating-substrate
interface, owing to differences in thermal expansion of both
208 D. Al-Anazi et al. / Journal of Materials Processing Technology 174 (2006) 204–210
Fig. 6. Coat cross-section and top view of coated surface after three-point bending tests.
materials, influences significantly adherence of coating to the
substrate material, despite the fact that gradual cooling in air
ambient was carried out.
Fig. 7 shows load–displacement curves obtained from the
experiment and simulation. It can be observed that both curves
are in agreement, which in turn lead to a realistic results for
stress and strain predictions.
Fig. 8 shows three von-Mises stresses corresponding to three
load conditions at coating substrate interface. It should be noted
that the first load condition corresponding to the elastic region
while second and third load levels are in the elasto-plastic and
plastic regions. In the elastic region, von-Mises stress is max-
Fig. 7. Force vs. displacement behavior obtained from three-point experiment
and used in the FEM (ANSYS) simulations.
imum at the point of maximum deflection of the workpiece.
The magnitude of the von-Mises stress is considerably less than
the elastic limit of the coating and substrate material. In the
case of high load levels, the maximum magnitude of von-Mises
stress extends along the horizontal direction with its magnitude
exceeding the elastic limit of the coating and base material. This,
in turn, results in multi-cracking of the coating within the region
of maximum deflection. This situation can also be observed from
Fig. 5. As the load level increases, von-Mises stress increases
sharply in the region of maximum deflection while extension of
high magnitude of von-Mises stress at coating interface contin-
ues. This causes elongated cracks to be formed in the coating in
the deflection region. Although stress realization at coating inter-
face is resulted due to elongated cracks, continuation of bending
load results in severe damage in the coatings such that partial
peel-off coating from the base material surface is resulted.
Fig. 9 shows total strain at three loading conditions at coating-
base material interface. At low loading situation (in the elastic
deflection region) total strain is highest at the region of deflec-
tion. The axial extension of the total strain is limited with the
maximum deflection region. As the load level increases (in
elasto-plastic region), total strain extends along the interface
in the horizontal direction, provided that maximum total strain
occurs in the location of maximum deflection. This indicates
that plastic deformation only occurs in the region limited with
the maximum deflection. As the load level increases further the
magnitude of strain reduces and the total strain reaches its peak
at the point of deflection. This suggests that formation of elon-
gated crack in the coating relieves the stress level in the deflection
region and the crack formed is not confined to the base mate-
rial. This situation is also observed from the SEM micrograph
(Fig. 6).
 D. Al-Anazi et al. / Journal of Materials Processing Technology 174 (2006) 204–210 209

Fig. 9. Equivalent total strain when force = 120 N. Equivalent total strain when
Fig. 8. von Mises stress at different load conditions.
force = 3000 N.
210 D. Al-Anazi et al. / Journal of Materials Processing Technology 174 (2006) 204–210
5. Conclusions
von-Mises stress excess of elastic limit at coating-base mate-
rial interface extends in the horizontal direction, which indicates
that the crack formation in coating is unavoidable. As the load
level increases, elongated cracks are formed in the coating, par-
ticularly in the region of maximum deflection. Once the cracks
are formed, stress relaxation at coating interface occurs, which
reduces the strain in this region and the cracks do not propa-
gate into the base material. Further increase in load level causes
severe cracking of coating and partial peeling off coating from
the base material surface is resulted.
Acknowledgements
The authors acknowledge the support of Dublin City Univer-
sity in Ireland and KFUPM in Saudi Arabia.
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