Surface & Coatings Technology 261 (2015) 289–294

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Surface & Coatings Technology

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

Effect of bond coat and post-heat treatment on the adhesion of air plasma
sprayed WC-Co coatings
F. Ghadami a,⁎, M. Heydarzadeh Sohi a, S. Ghadami b
a
School of Metallurgy and Materials, College of Engineering, University of Tehran, Tehran, Iran
b
College of Engineering, Semnan University, Semnan, Iran

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

Article history: In this study, WC-12wt%Co and NiCr feedstock powders were sprayed by the air plasma spray (APS) method to
Received 31 July 2014 form conventional WC-Co and double-layer NiCr/WC-Co coatings on steel substrates. The microstructure of as-
Accepted in revised form 5 November 2014 sprayed samples with and without NiCr bond coat was analyzed and found to consist of WC, W2C and an amor-
Available online 13 November 2014
phous phase. The conventional WC-Co coating samples were also heat treated at 650, 900 and 1150 °C for 1 h.
Heat treatment at all temperatures examined resulted in phase changes within the coating layer by formation
Keywords:
WC-Co
of WxCoyC, η-carbides. Adhesive strength of the as-sprayed and heat-treated coatings also investigated. Results
NiCr bond coat indicated that adhesive strength has improved by applying bond coat before spraying of overlay WC-Co coating.
Interface The results also showed that by increasing heat treatment temperature from 900 °C to 1150 °C, adhesive strength
Heat treatment increased. In this case, post-heat treatment process at 1150 °C and or applying NiCr bond coat gave the higher
Adhesive strength adhesive strength, which was due to the control of interfacial porosities and formation of partially metallurgical
bonding in interface of coating and substrate.
© 2014 Elsevier B.V. All rights reserved.

1. Introduction may increase the adhesive strength of the resultant coating by reducing
stresses in the coating, which are caused by thermal expansion differ-
WC-Co composite coatings are commonly used to enhance the wear ences of the coating relative to the substrate material [10].
resistance of many types of engineering components. It is common Therefore, the adhesion of plasma sprayed WC-Co coating is usually
practice to deposit WC-Co coatings by thermal spray techniques such improved with the improvement in the degree of particle melting be-
as air plasma spray (APS) and high velocity oxygen fuel (HVOF) [1–5]. cause good melting leads to a better flattening and/or using a suitable
To meet the tribological requirements, the coated materials must bond coat layer, which provide a suitable base for overlay coating [2,11].
possess a suitable combination of properties and adhesion of coating Different post-treatments such as laser treatment, hot isostatic
on the substrate is one of them. The adhesion of plasma sprayed WC- pressing (HIP) [12,13], spark plasma sintering (SPS) [14] and heat
Co coating depends on spraying system, spraying parameters, powder treatment processes in vacuum or inert gas [15,16] are recommended
morphology, residual stresses in coating, roughness of substrate and for improving the quality and adhesion of WC-Co coatings. Post-heat
type of bond coat (if exists) before WC-Co deposition. If adhesion of treatment process of WC-Co coatings, increases the effective carbides
WC-Co coating on a part is not sufficient during the exploitation time, content (with higher hardness and wear resistance) due to the recrys-
coating may pull out; therefore, failure in mechanism occurs [6]. tallization of the amorphous phases in the coating to η-carbides [15,
During plasma spraying, WC-Co particles, during their flight due to 17–19]. η-Carbides are commonly formed in WxCoyC ternary system
surface tension, are considerably deformed upon hitting the substrate.
Li et al. [7] believe that the adhesion of a thermally sprayed coating
deposited by completely molten droplets is mainly achieved by the
mechanical interlocking effect except the deposition of refractory mate- Table 1
rials. This is because the deposition of refractory materials may cause Powder feedstock characteristics.
the local melting of steel substrate for example [8], which consequently Characteristics WC-Co coating NiCr bond coat
leads to the metallurgical bonding [7,9].
Powder size (μm) −53 + 11 −125 + 45
Berndt [10] reported that some chemical reactions may occur be- Manufacturing process Agglomeration and Sintering Cast and crashed
tween the bond coat and steel substrate. In addition, the bond coat Powder morphology Spherical and semi-sphere Clad
Manufacturer company TAFA-Praxair® Metco®
Powder specification 1324VM/WC727-1 Metco 444
⁎ Corresponding author. Tel.: +98 912 5333626; fax: +98 21 88006076.
Flow density (g/mm3) 4.2 4.2
E-mail address: farzin.ghadami@gmail.com (F. Ghadami).

http://dx.doi.org/10.1016/j.surfcoat.2014.11.016
0257-8972/© 2014 Elsevier B.V. All rights reserved.
290 F. Ghadami et al. / Surface & Coatings Technology 261 (2015) 289–294

Table 2 coatings. APS process for both bond coat and overlay coatings were car-
Spray parameters employed during APS process for overlay coating and bond coat layer. ried out in an Ar/H2 plasma gases.
Parameter WC-Co coating NiCr bond coat Table 2 lists the important spray parameters employed for WC-Co
Nozzle diameter (mm) 6 6
coating and NiCr bond coat. The samples were grit blasted for cleaning
Plasma gas flow Ar (l/min) 65 65 and roughening of the surfaces before coating. All specimens were
Secondary gas flow H2 (l/min) 3 14 mounted on the circumference of a horizontally rotating turntable and
Carrier gas Ar (l/min) 2 2.3 cooled during and after spraying with compressed air jets. The plasma
Arc current (Amp) 700 600
gun was attached to a transverse unit controlling the vertical move-
Arc voltage (V) 58 63
Spraying angle 90° 90° ment. In this case, the rotating speed was 120 rpm (0.8 m/s of linear
Powder feed rate (g/min) 36 40 speed) and vertical transverse speed was chosen 0.15 m/s.
Stand off distance (mm) 140 140
Digital setting 40 40 2.3. Post-heat treatment process

The heat treatments were carried out in an inert atmosphere to pre-

which consists of one or a combination of W3Co3C, W4Co2C and W6Co6C vent oxidation of both the coating and substrate. Single-layer WC-Co
[17]. coating samples (without bond coat) were placed in a furnace which
The object of this paper is the effects of NiCr based bond coat and was filled with argon before being heated at 20 °C min−1 up to the treat-
heat treatment process on adhesive strength of air plasma sprayed ment temperature. They were then held for 1 h before being allowed to
WC-12wt%Co coatings were investigated. cool to room temperature in the furnace. The heat treatment tempera-
tures were chosen at 650 °C, 900 °C and 1150 °C.
2. Experimental
2.4. Coatings characterization
2.1. Coating materials
A Phillips™ 5300JPL scanning electron microscope (SEM) was used
for structural characterization of the coating before and after heat
The agglomerated and sintered WC-12wt%Co feedstock powder
treatment. ImageTool (ver 1.2) analyzer software was utilized for inter-
obtained from TAFA-Praxair® (1324VM) was used as overlay WC-Co
pretation of interfacial porosity distribution. The crystalline phases of
coating. In addition, clad Ni-9wt%Cr-5wt%Al-5.5wt%Mo-5wt%Fe
as-sprayed and heat-treated deposits were identified using X-ray
Sulzer-Metco® (Metco444) powder was applied as NiCr based interlay-
diffraction (XRD), and measurements were made on an x'pert Phillips™
er bond coat. In this case, substrates were chosen mild steel (0.23wt%C).
diffractometer with Cu-Kα (λ = 0.15406 nm) radiation at 40 kV and
The main characteristics of overlay and bond coat powders used are
30 mA. A low scanning rate of 0.2 °/min was used to achieve the desired
given in Table 1.
precision.

2.2. Air plasma spraying process 2.5. Adhesive strength of the coatings

A3000 APS equipment (Plasma-Technik®, Switzerland) was used to Tensile adhesion tests (TAT) were carried out in accordance with
deposit 30 μm thickness of NiCr bond coat and 200 μm of WC-Co overlay ASTM C633 standard test for as-spayed and heat-treated WC-Co

Fig. 1. Tensile adhesion test (TAT) for WC-Co and NiCr/WC-Co-coated specimens according to ASTM C633.
 F. Ghadami et al. / Surface & Coatings Technology 261 (2015) 289–294 291

Fig. 2. Backscattered electron micrograph of as-sprayed WC-Co coating: (a) coating layer, (b) interface zone, (c) interfacial porosity distribution and also WC-Co coating with NiCr bond
coat, (d) coating layer, (e) interface zone and (f) interfacial porosity distribution.

coatings and then compared with WC-Co coating with NiCr bond coat
(NiCr/WC-Co coatings). The test specimen consisted of a pair of mild
steel cylindrical stubs, 25.4 mm (1 inch) in diameter and height. A
pair of test stubs, one plasma sprayed coated specimen and the other
uncoated but grit blasted and degreased, were bonded together with
3 M Scotch weld™ SW-2214 adhesive to form the tensile bond strength
test specimen. Then they were pulled to fracture in a screw-driven uni-
versal testing machine at a displacement rate of 1 mm min-1 (Fig. 1).

3. Results and discussion

3.1. Characterization of the coatings and interfaces

Fig. 2 shows the SEM microstructure of cross section of as-sprayed

WC-Co and NiCr/WC-Co coatings. Both types of coatings display the
usual banded microstructure typical of thermally sprayed WC-Co
coatings. This figure illustrates that two distinct matrix and carbide
types are present in overlay in both types of coating. In addition, WC-
Fig. 3. Adhesive strength versus heat treatment temperature for as-sprayed and heat- Co coatings layer have lamellar structure and consist of two major
treated WC-Co coatings as compared with NiCr/WC-Co coating. phases, carbide phase and cobalt rich matrix phase, together with
292 F. Ghadami et al. / Surface & Coatings Technology 261 (2015) 289–294

According to Lim et al. [20], dispersed micro-cracks may form in in-

terface zones for coatings heat-treated at 650 °C. It is obvious that dur-
ing the TAT test, these micro-cracks can propagate and link together to
form a fatal crack that finally reduced the bond strength of the treated
coating as compared with as-spray coating.
Furthermore, interdiffusion of cobalt (Co) in the coating and iron
(Fe) in the substrate may occur and causes metallurgical bonding be-
tween coating and substrate [16]. This phenomenon probably starts to
form and accelerate at higher heat treatment temperatures (above
900 °C) by accelerating interdiffusion process in coating/substrate inter-
face [19,20]. On the other hand, sufficient interfacial diffusion and the
precipitation of η-carbides can overcome to the crack propagation at
higher heat treatment temperatures [20]. Therefore, post-heat treat-
ment of WC-Co coatings at 900 °C and 1150 °C increased adhesive
strength.
Fig. 4 presents fractured surface images of the coated specimens be-
fore and after heat treatment as compared with NiCr/WC-Co coating.
For as-sprayed WC-Co-coated specimen, about 75% of coating layer de-
tached from interface (A) and 25% of coating remains (B) with 57 MPa
adhesive strength after TAT (Fig. 4a). In this case, for heat-treated spec-
Fig. 4. Coating detachment after TAT process for (a) as-sprayed WC-Co, (b) heat treated at imens at 650 °C and 1150 °C, 85% of coating detachment (A) occurs in
650 °C, (c) heat treated at 1150 °C and (d) as-sprayed NiCr/WC-Co.
46 MPa, and 60% of coating detachment (A1 + A2) occurs in 63 MPa
(Fig. 4b and c). In comparison, it's clear that a cohesive failure has de-
interlamellar pores and microporosities (Fig. 2a and d). In Addition, as tected for NiC/WC-Co in 65 MPa. For WC-Co-coated specimen heat
compared with WC-Co coating, it can be seen that NiCr bond coat ad- treated in 1150 °C (at the maximum adhesive strength), the fracture
heres well to substrate for NiCr/WC-Co coating specimen and in turn in bright zones (A1) and dark zones (A2) has happened within the coat-
provides an excellent surface for WC-Co overlay (Fig. 2b and e). Interfa- ing/substrate interface. At the zone B, on the other hand, the detach-
cial porosity distribution for WC-Co and NiCr/WC-Co coating specimens ment has occurred in adhesive material (Fig. 4c).
also shown in Fig. 2c and f. A sort of weak mechanical bonding with In the same case, Fig. 5 shows SEM image of coating/substrate de-
partially coarse porosity distribution are presented in WC-Co/ tached surface, after TAT process for WC-Co coating after heat treatment
substrate interface as compared with NiCr/WC-Co and NiCr/substrate at 1150 °C. From this figure, it is clear that two major regions are detect-
interfaces which has fine and well-distributed porosities. It can be able. These areas consist of bright region (A1) in which coating remains
seen that NiCr bond coat layer has improved mechanical contact be- in the substrate and dark region (A2), which presents roughened blast-
tween overlay WC-Co coating and steel substrate and hence decreased ed steel substrate. Energy-dispersive X-ray spectroscopy (EDS) analysis
porosity in interface zone. of bright (A1) and dark (A2) regions of detached WC-Co coating heat
treated at 1150 °C after TAT test, are presented in Fig. 6. From this figure,
it can be seen that W, Co and Fe peaks are presented in bright region
3.2. Adhesive strength of the coatings (A1), which confirms intermetallic components in coating layer near
the interface (Fig. 6a). EDS analysis of dark region (A2) also showed
Fig. 3 shows tensile adhesive strength of the WC-Co coatings as a Fe, Co and Al traces in substrate near the interface. The detection of Co
function of heat treatment temperature together with NiCr/WC-Co ad- peaks in substrate may confirm that the inter-diffusion of Co element
hesive strength. Except for the coating heat treated at 650 °C, heat treat- forms coating layer into steel substrate, which results in partial metal-
ment of the coated samples results in increasing adhesive strength. lurgical bonding in WC-Co coating after heat treatment at 1150 °C. In
Results also indicated that NiCr bond coat layer improved adhesive addition, probably because of trapping of some very fine blasting alumi-
strength for NiCr/WC-Co coating specimen. na particles (Al2O3) on roughened substrate surface during sand

Fig. 5. (a) Scanning electron micrograph of failure through the coating/substrate interfacial region for WC-Co coating specimen heat treated at 1150 °C after TAT process consisting bright
(A1) and dark (A2) regions. (b) Failure through the coating/substrate interfacial region at higher magnification.
 F. Ghadami et al. / Surface & Coatings Technology 261 (2015) 289–294 293

Fig. 6. EDS analysis of interface region for detached WC-Co coating heat treated at 1150 °C after TAT process, (a) bright region (A1) and (b) dark region (A2).

blasting before coating process, Al peaks are presented in EDS analysis heat-treated coatings in 900 °C and 1150 °C show peaks indexed to
of roughened substrate in A2 region (Fig. 6b). η-carbides (W3Co3C, W4Co2C and W6Co6C). The XRD spectra for the
At present, there is some contention about the precise mechanisms samples heat treated above 900 °C showed traces where the η-carbide
for the high adhesion of the bond coat and also why intermediate NiCr peaks were narrow and of comparable height to the WC and W2C.
coating confers high adhesion to the WC-Co overlay. The explanation Diffraction patterns of the heat-treated coatings did not show any amor-
is that the NiCr bond coat readily melts and flows at the substrate phous phase especially in 1150 °C. XRD spectra for bond coat interface
surface and therefore imparts a high specific area of contact which pro- zone for heat-treated WC-Co at 1150 °C show Co3Fe7 intermetallic
motes good adhesion [21]. On the other hand, the NiCr bond coat may phase together with WC, W2C and η-carbides. This intermetallic com-
act as a compliant layer between the steel substrate and WC-Co overlay pounds maybe formed because of chemical reaction or metallurgical
so that may increase the adhesive strength by reducing stresses bonding in bond coat/substrate interface which confirms increasing ad-
between the coatings and substrate [10]. hesive strength for WC-Co coatings after heat treatment above 900 °C.
Fig. 7 shows the X-ray diffraction spectrum of the conventional
agglomerated and sintered WC–Co powder feedstock, together with 4. Conclusions
as-sprayed, coating heat-treated WC-Co at 1150 °C and NiCr/WC-Co in-
terface zone. The XRD spectra for the feedstock powder show peaks NiCr and WC–12wt%Co powders were deposited onto steel
indexed to WC and Co. The XRD traces of the as-sprayed coatings exhibit substrates to form single-layer WC-Co and double layer NiCr/WC-Co
WC and W2C peaks along with broad diffuse peaks (humps) between coatings by APS method. Single WC-12wt%Co coatings were heat
2θ = 37 ~ 46° and 2θ = 73 ~ 81° representing amorphous or nanocrys- treated at 650 °C, 900 °C and 1150 °C for 1 h in a controlled atmosphere.
talline material. These results have also been reported by Sohi and The structural properties and adhesive strength of the as-sprayed and
Ghadami [18] and Stewart et al. [15]. Owing to decarburization and heat-treated coatings were studied and compared with NiCr/WC-Co.
dissolution of the WC in liquid cobalt at high temperatures [19] and The results are summarized as follows:
thermal and kinetic history of melted particles, the phases present in
the coating differ from those in the powder. Diffraction patterns from • The as-sprayed WC-Co coatings consisted of WC, W2C and an amor-
phous phase including cobalt, tungsten and carbon.
• Post-heat treatment of WC-12wt%Co coatings in an inert atmosphere
above 900 °C promoted the formation of η-carbides (W3Co3C, W4Co2C
and W6Co6C) from the amorphous phase.
• By applying NiCr bond coat, adhesive strength of NiCr/WC-Co has
increased by decreasing interfacial porosities that promotes good ad-
hesion in coating/bond coat and bond coat/substrate interface zones.
• Heat treatment at 900 °C and 1150 °C increased the adhesive strength
of WC-12wt%Co coating layer, which could be due to the formation of
partially metallurgical bonding between coating and substrate.

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