Surface and Coatings Technology 184 (2004) 208–218

Adhesion testing of thermally sprayed and laser deposited coatings

¨
Anders Hjornhede, Anders Nylund*
¨
Department of Materials Science and Engineering, Chalmers University of Technology, SE – 412 96 Goteborg, Sweden

Received 3 June 2003; accepted in revised form 3 November 2003

Available Online 27 February 2004

Abstract

Commercial coatings were deposited on low-alloyed steel tubes (Fe1Cr0.5Mo) by arc spray, HVOF (high velocity oxy fuel)
and laser cladding. The adhesion strength was tested with two methods: acoustic emission and a combination of four point
bending and metallography. The agreement between the results obtained from the two different experimental techniques is very
good. Laser coatings showed no delamination for strains up to 15%, while coatings deposited with the arc spray and HVOF
processes delaminated in the strain intervals 1.4–1.9% and 0.8–1.8%, respectively. The suggested delamination mechanism is the
initial formation of a radial crack in the coating after which the coatingysubstrate interface comes under an increased tension load
and fractures. Arc sprayed coatings of Metcoloy 2 (Fe13Cr) mixed with the binder 80Ni20Al show a strongly improved adhesion
strength if the splat size is sufficiently large. The delamination interval increases to 10.5–11.5%. However, for small splats the
effect is eliminated.
䊚 2003 Elsevier B.V. All rights reserved.

Keywords: Thermal spraying; Laser coating; Acoustic emission; Adhesion testing

1. Introduction cladding has been introduced since lasers have become

Components in combustion fluidised beds are sub-
jected to erosion–corrosion due to erosive bed particles
and corrosive species in the gas phase. The degradation
rate of low–alloyed steels in such environments is not
acceptable. The use of thicker equipment walls and
high–alloyed steels prolongs the lifetime of the com-
ponents but at the expense of a high physical weight
and cost. An alternative solution is to cover low–alloyed
steels with an erosion–corrosion resistant coating. Tra-
ditionally, thermal spray methods like electric wire arc
spray have been used due to the simple processing and
low cost w1x. The technique also has the advantage that
it makes the possibility of in-situ coating during service
and repair possible. A more novel method is high
velocity oxygen fuel (HVOF) where the use of powder
results in denser coatings, lower oxide contents and a
wider range of possible coating materials, including
carbides and ceramics w2x. As a third alternative, laser
*Corresponding author. Tel.: q46-31-7721263; fax: q46-31-
7721313.
E-mail addresses: anders.nylund@me.chalmers.se (A. Nylund),
anders.hjornhede@me.chalmers.se (A. Hjornhede).
¨ acoustic emission (AE) where the initiation and devel-
more sophisticated, smaller and cost effective. The main
advantages of the laser coatings are their strong adhesion
to the substrate and their low porosity and oxide content
w3 x .
To obtain the optimum quality of an applied coating,
the degradation rate in the chemical environment must
be minimised and the adhesion strength to the substrate
maximised. Due to different thermal expansion coeffi-
cients for the coating and substrate, material stresses are
induced when coated components are used in high
temperature applications. The stresses are intensified by
temperature gradients originating from the temperature
difference between the temperatures of the fire and the
steam sides of the coated tubes. Further, in the case of
power plants temperature fluctuations during service,
expose the coated surfaces to thermally induced strains
with an increased risk of delamination. The adhesion
strength of coatings is traditionally evaluated by tensile
testing, e.g. ASTM C 633 or bending tests followed by
metallography w1x. However, these methods have the
drawback of requiring optical investigations to identify
the induced damages. An option would be the use of

0257-8972/04/$ - see front matter 䊚 2003 Elsevier B.V. All rights reserved.
doi:10.1016/j.surfcoat.2003.11.008
 ¨
A. Hjornhede, A. Nylund / Surface and Coatings Technology 184 (2004) 208–218 209

Table 1
The composition of the coatings used in this study

Coating Composition (wt.%)

Arc spray
Metcoloy 2 Fe12.4Cr0.6Ni0.4Mn0.4Si0.36C
(Air or N2, small splat size)
80Ni20Al-binder, 80Ni20Al
(Air, small splat size)
Metcoloy 2q80Ni20Al. (Air 50 (Metcoloy 2)q50 (80Ni20Al)
or N2, large splat size)
Metcoloy 2q80Ni20Al-binder. 50 (Metcoloy 2)q50 (80Ni20Al)
(Air, small splat size)
HVOF
Metcoloy 2 Fe12.4Cr0.6Ni0.4Mn0.4Si0.36C
Amperit 526 83WC17Co
Metco 3007 80Cr3C2 –16Ni4Cr
Laser
Metcoloy 2 Fe12.4Cr0.6Ni0.4Mn0.4Si0.36C
Inconel 625 Ni21.5Cr9.0Mo3.6Nb2.5Fe0.3Si0.05C
Duroc 5177 Ni26.8Cr8.4Mo1.7Fe1.40C0.9Nb0.7Si
Duroc 17=1% C Ni25.0Cr8.8Mo1.9Fe1.9Nb1.00C0.7Si
Stellite 6 Co28.5Cr4.2W1.1C1.0Si-2.0Ni-1.5Fe
Stellite 21qTiC 85(Co27.0Cr5.5Mo2.8Ni0.9Si0.25C-2.0Fe)q15(Ti19.4C)
Duroc 5177qTiC 85(Ni26.8Cr8.4Mo1.7Fe1.40C0.9Nb0.7Si)q15(Ti19.4C)
Duroc 17=1% CqTiC 85(Ni25.0Cr8.8Mo1.9Fe1.9Nb1.00C0.7Si)q15(Ti19.4C)
Stellite 6qTiC 85(Co28.5Cr4.2W1.1C1.0Si-2.0Ni-1.5Fe)q15(Ti19.4C)

opment of cracks is continuously monitored during the
tensile testing. The technique has been successfully
applied to plasma sprayed coatings, carbon fibre mate-
rials, composites, thermal barrier coatings and hard metal
coatings w4–9x. The aim of this paper is to further apply
the method of acoustic emission and use it for analysing
the adhesion of metallic coatings on a substrate of low-
alloyed steel tubes. The results are compared with those
from traditional testing techniques.
2. Experimental
2.1. Raw materials and coating production
The adhesion strength of coatings deposited with laser,
HVOF and arc spray (air or N2 as carrier gas) was
tested. The thermally sprayed coatings were deposited
in accordance with the recommendations given by the
suppliers, with the exception of the large splat coatings,
where the parameters were slightly altered. The deposi-
tion parameters used in the laser process are not allowed
to be published. The coatings and their chemical com-
positions can be seen from Table 1.
Metcoloy 2 (wire) and Metco 3007 (powder) are
standard products manufactured by Sulzer Metco. The
powder with the same composition as Metcoloy 2 but
used for the HVOF and laser deposition techniques were
¨
manufactured by Hoganas ¨ AB. The Amperit 526, Stellite
6 and 21, Inconel 625 and Duroc materials were manu-
factured by H.C. Starck GmbH, Deloro Stellite, Special
Metals Corp. and Duroc Energy AB, respectively. The
size grades for the powder used with laser and HVOF
were 63–150 mm and 5–63 mm, respectively. The
thicknesses of the coatings were in the range 0.7–1.2
mm for laser, 0.4–0.6 mm for arc spray and 0.2–0.4
mm for HVOF. As substrate, steel tubes of a type
normally used in high-pressure applications,
Fe0.1C1Cr0.5Mo0.5Mn0.2Si, were chosen. The surface
roughness of the arc sprayed and HVOF deposited
substrate tubes was 5–7 mm and 10 mm, respectively
(Ra-values). The Metcoloy 2 and 80Ni20Al materials
were supplied as the two separate electrodes in the arc
spray process, resulting in a coating consisting of 50%
of each material. Two different arc spray droplet sizes,
50 and 200 mm, were examined for the Metcoloy 2q
80Ni20Al-coating.
The adhesion of the coatings to the substrate was
tested with the three methods as described below; a
specially designed tensile test, a four-point bending test
followed by metallography and a four-point bending test
combined with acoustic emission (AE).
2.2. Tensile testing
The adhesion of the coatings to the substrate was
tested according to a tensile testing method developed
from the ASTM 633 test. The modified design was used
in order to simulate the tube geometry. A 10=15 mm
string coating was deposited on the tubes (external
diameter 33.7 mm, wall thickness 3.6 mm and length
210 ¨
A. Hjornhede, A. Nylund / Surface and Coatings Technology 184 (2004) 208–218
Fig. 1. Adhesion testing; experimental set-up for the tensile test.
approx. 20 mm). A cylinder (external diameter 8.0 mm)
with the same curvature as the envelope surface of the
tube was glued on top of the coated string, Fig. 1. The
tensile strength of the glue used, FM-1000䉷, is 69 MPa
after hardening. Peeling forces caused by misaligned
attachment of the cylinder were reduced by using a
brace designed as a hook and equipped with a spherical
prong. A total of 54 samples were tested.
2.3. Four-point bending test combined with metallogra-
phy and acoustic emission analysis
2.3.1. Experimental setup
The experimental set-up is illustrated in Fig. 2a. The
dimensions of the tubes used in this test were the same
as in the tensile test except for the length, which was
300 mm. A 100=10 mm wide coating was deposited
in the axial direction of the tubes and then subjected to
four-point bending at a displacement speed of 0.25 mmy
min. The displacement was measured with a position
gauge centred on the coating surface. The distances
Fig. 2. (a) Adhesion testing; experimental set-up for the four point bending and acoustic emission tests. (b) Scooped supports used in the four-
point bending test.
between the supports and the load applicators were 250
mm and 25 mm, respectively. All cylindrical supports
and load applicators were scooped to the same radius
as the tubes, Fig. 2b, and MoS2 was supplied in the
scoops before the tests in order to reduce the fretting.
Due to the tube geometry the test is not a pure four-
point bending test. Rather the stress load is described as
a parabola with its maximum between the two load
applicators.
2.3.2. Strain calibration
In order to determine the strain as a function of the
displacement, five strain gauges were glued on uncoated
tubes in the same area as the coating. One strain gauge
was positioned at the centre of the assumed coating
area, two at a distance of "5 mm off centre in the
radial direction, and two at a distance of "15 mm off
centre in the axial direction. The tubes were then bent
to different displacements. The largest strain was always
measured in the central position. This was then used to
establish a calibration curve from which the displace-
ments applied to the coated tubes were translated into
strain. The presence of a coating on the surface will
influence the strain distribution somewhat. In the case
of thermally sprayed coatings, the influence is limited
due to the relatively low adhesion strength. Further, in
a comparative study, like this, the deviation is about the
same among the coatings. The influence on the laser
coatings is larger, but due to the complex deformation
in the coated area of the tube, no adjustments were
done. The absolute displacement among the experiments
was adjusted in order to identify the strain at which
coating delamination was initiated, meaning that several
tests on each material were needed. After bending, an
80-mm long section was cut from the centre of the
deformed tube and divided into two pieces at the
position corresponding to the centre line of the coating,
Fig. 3. Each piece was then polished on emery paper
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A. Hjornhede, A. Nylund / Surface and Coatings Technology 184 (2004) 208–218
Fig. 3. The sectioning procedure of the bent tube for delamination
analysis.
and diamond paste after which the delamination length
was measured with optical microscopy. A total of 69
tubes were tested.
2.3.3. Acoustic emission analysis
Two piezo electrical acoustic emission sensors (Phys-
ical Acoustic Corporation (PAC), R15 resonance fre-
quency 150 kHz) were attached at the ends of the coated
tubes with the full active area joined to a brass device,
pinched on the tubes and tightened with a screw, Fig.
2a. Dow Corning䉷 high vacuum grease was used as
couplant between the sensor and the pinch device. The
sensor positions were chosen for minimising acoustic
emission emerging from deformation of the tube. The
frequency response of the sensors is roughly 50–520
kHz for transient (burst) signals. This overlaps with the
results, which have shown that 90% of the acoustic
emission emerging from material deformation is within
the frequency band of 10–550 kHz w9x. The sensors are
connected to an amplifieryfilter with a gain of 40 dB.
The amplifiers are in turn connected to an eight bit deep
sampling resolution ISA AyD-converter card. One event,
or 16 384 samplesychannel (a waveform) is sampled
whenever a trigger event occurs and then transferred to
the computer, giving a dead time of approximately 20
ms. The sampling rate was set to 5 MHz. The energy
of the acoustic emission for one event was calculated
16384
as Es 8 Ui2(U; voltage generated in the piezoelectric
i
crystal due to the emitted acoustic emission) and then
accumulated event by event. Software written in Lab-
Table 2
Summary of the ASTM 633 tensile tests on the different coating types
Coating method
Laser
HVOF
Arc spray
211
View recorded the events as a function of the displace-
ment at the centre of the tube. No analyses were
performed in real time.
In order to obtain the acoustic emission originating
from deformation of the tube, the supports, the load
applicators, the tensile testing machine and other uni-
dentified sources, uncoated tubes were tested and used
as reference. Only signals reaching both sensors were
analysed and calculations made from the signal travel-
ling time showed that the vast majority of the acoustic
emission recorded originated from the volume below
the two load applicators.
2.4. Microstructural investigations
Polished cross-sections of the coatings were examined
in an optical microscope after the testing. The coating
hardness was measured with Vickers method. The com-
position of selected areas on some coatings was deter-
mined by Auger spectroscopy (PHI 660), from which
also the SEM-imaging capabilities were used.
3. Results
3.1. Tensile testing
The results obtained from the tensile testing are
summarised in Table 2 and the failure mechanisms are
schematically illustrated in Fig. 4.
In the tests performed with laser coatings, the glue
fractures show that the adhesion strength of the coating
exceeds 69 MPa. In contrast, coatings deposited with
the HVOF technique delaminated at the coatingysub-
strate interface. Arc sprayed coatings did not delaminate
due to internal fracture at a stress of approximately 38
MPa, implying that in this case the adhesive strength
exceeds the cohesive strength. No significant differences
were noted among the various arc sprayed coatings. The
results from this study clearly show that adhesion failure
is only obtained for the HVOF coatings. Thus, the
tensile testing method is not applicable for laser and arc
spray coatings.
3.2. Bending test in combination with metallography
Fig. 5 shows a cross section of the Metcoloy 2 coating
deposited with laser. The microstructure is very uniform
Tensile strength
Various coatings. The tensile strength exceeds 69 MPa (4 tests)
Amperit 526 and Metco 3007: 55"10 MPa (5 tests and 4 tests, respectively)
Metcoloy 2: 61"7 MPa (4 tests)
Various coatings. 38"12 MPa. (23 tests)
212 ¨
A. Hjornhede, A. Nylund / Surface and Coatings Technology 184 (2004) 208–218
Fig. 4. Bonding failure mechanisms of the three different coating types
as obtained with the tensile testing.
with a low porosity and oxide content. No signs of
delamination were seen even after bending to strains as
large as 15%. However, radial cracks occurred on a
small number of samples after the bending procedure.
These cracks cannot be linked to the composition or
thickness of the coating.
A dozen bending tests were performed on Metcoloy
2 coatings arc sprayed in air to find the strain at which
delamination is initiated. The length of any delamination
was measured for both the sectioned sample pieces.
Summarising gives the maximum delamination length
as 160 mm. Fig. 6a shows the microstructure of a
sample bent to a strain of 0.5%. No cracks or signs of
delamination are seen. The coating consists of many
layers of overlapping essentially lamellar particles, drop-
lets, which are sometimes called splats. Compared to
the laser coating the oxide content and degree of porosity
is much larger w10x. The same material at a strain of
1.25% is shown in Fig. 6b. A radial crack has formed
in the splat boundaries and isolated areas of delamination
have nucleated at the coatingysubstrate interface. The
total delamination length is 2 mm in this case. At a
stress of 1.9% a relatively large radial crack and a
massive delamination (32 mm in this case) is seen, Fig.
6c. Delamination without radial cracks perpendicular to
the coatingysubstrate interface has not been observed
on the thermally sprayed coatings. However, coatings
with only small radial cracks and no delamination have
been observed.
The delamination process is similar for HVOF
sprayed coatings. Fig. 6d shows the microstructure of
an HVOF-sprayed Metcoloy 2 coating after bending to
a strain of 2.1%. For this type of coating, partially
developed radial cracks are never observed and radial
cracks without delamination are very rare. This implies
that delamination occurs immediately after formation of
a radial crack.
Figure 7 shows the delamination length as a function
of strain for some selected materials and coating meth-
ods. Metcoloy 2 arc sprayed in air starts to delaminate
at a strain of approximately 1.4%. From the same coating
material but arc sprayed in nitrogen gas, only three
points are available. It is seen that delamination has
occurred at a strain of 1.8%. Mixing the bond coat
material 80Ni20Al into the Metcoloy 2 coatings increas-
es the adhesion strength dramatically, if the splat size is
sufficiently large. Application of strains as large as 10–
15% just gives a minor delamination. However, it is
clearly seen that the effect is negligible for small splats.
The HVOF sprayed coating, (Metco 3007) shows worse
adhesion compared to the arc sprayed ones. Delamina-
tion is initiated already at a strain of approximately 1%.
Metcoloy 2 coatings deposited with laser do not delam-
inate at all, not even for strains up to 15%. The results
show that, with the exception of the Metcoloy 2q
80Ni20Al coatings with a large splat size, the delami-
nation rate is very high as soon as delamination is
initiated.
In Fig. 8, the strain interval at which delamination is
initiated is shown for all thermally sprayed coatings.
The lower end of each column corresponds to the largest
strain where no signs of delamination have been
observed and the higher end corresponds to the lowest
strain at which delamination has been observed. The
Amperit 526 coatings were subjected to a maximum
strain of 1.5% and did not delaminate while the other
two HVOF coatings, Metco 3007 and Metcoloy 2,
delaminated at a strain of 1.0–1.5% and below 2%,
respectively. Delamination of the Metcoloy 2 coatings
Fig. 5. Cross section of laser coated Metcoloy 2 (optical microscopy).
 ¨
A. Hjornhede, A. Nylund / Surface and Coatings Technology 184 (2004) 208–218 213

Fig. 6. Cross section of Metcoloy 2 coating, arc sprayed in air at (a) 0.5%, (b) 1.25% and (c) 1.9% strain. (d) Cross section of HVOF sprayed
Metcoloy 2 coating at 2.1% strain (optical microscopy).

deposited with arc spray starts in the same strain region the bending machine and should be considered when
as for the Metco 3007 coating; between 1.1–1.25% for evaluating the tests performed with coatings. The behav-
those sprayed in air and 0.5–2.1% for those sprayed in iour of an Inconel 625 laser coating is similar to the
nitrogen gas. Addition of 80Ni20Al clearly increases the
delamination region for Metcoloy 2 coatings to the
strain interval 2.2–10%. However, if the splats do not
have a sufficient size the effect of the binder disappears
as seen from columns 8 and 9 in the figure.

3.3. Bending test in combination with acoustic emission

monitoring

During all bending tests the acoustic emission was

simultaneously recorded. The results from the coatings
were normalised by the same amplifying factor as for
the reference. In Fig. 9, the normalised accumulated
energy is shown as a function of strain for some selected
coatings. Results from a reference test on an uncoated
tube shows an initial sharp rise in acoustic emission at
a strain of 0.1–0.25% after which the curve has a
continuous slope with a small inflexion at a strain of
approximately 2%, Fig. 9c. The sources of acoustic
emission in this case are deformation of the tube, fretting Fig. 7. The delamination length as a function of strain for selected
against the supports and load applicators and noise from coatings.
214 ¨
A. Hjornhede, A. Nylund / Surface and Coatings Technology 184 (2004) 208–218

Fig. 8. The strain intervals where delamination is initiated on thermally sprayed coatings. The figures in the columns indicate the number of
tested samples for each coating quality. The number on the x-axis corresponds to the one given in the legend denoting the coating materials.

reference tube, Fig. 9c, with a sharp increase in energy
level at 0.1% strain and an inflexion at 2% strain. This
indicates that the acoustic emission activity originates
from deformation of the tube and not from the laser
coating. The coating did not delaminate for strains up
to 15% and the energy increase at larger strains is
therefore only due to further deformation of the tube,
Fig. 9a. However, in the case when radial cracks occur
(only in a few laser coatings) an instant rise in the
accumulated energy level takes place (not shown here).

Fig. 9. (a) Accumulated acoustic emission energy vs. strain. (b) Magnification of the region surrounded by a dashed ellipse in Fig. a. (c)
Magnification of the region surrounded by a continuous ellipse in Fig. b.
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A. Hjornhede, A. Nylund / Surface and Coatings Technology 184 (2004) 208–218
Bending of Metcoloy 2 coatings deposited with
HVOF or arc–sprayed with nitrogen or air, respectively
initially shows the same acoustic emission behaviour as
the reference tube. However, in the strain interval 1.2–
2% a sharp increase in accumulated energy level is
observed, Fig. 9b,c. The delamination length for the
coating arc sprayed in air at 1.9% strain, where the
experiment was terminated, is 32 mm, corresponding to
21% delamination. Sectioning of the sample deposited
with the HVOF-technique showed that the coating
delamination was complete. The sharp increase in accu-
mulated energy therefore indicates the formation of
radial cracks and subsequent delamination. The small
steps in energy increase approximately 1.4, 1.6 and
1.75% strain as seen in Fig. 9c might indicate formation
of radial cracks. The Metcoloy 2 coating arc sprayed in
nitrogen gas was run to complete delamination during
straining to 15%, Fig. 9a. In this case, the stepwise
behaviour is not observed. Instead, the increase in
acoustic emission activity starts at a strain of 1.9% and
decays at a strain of approximately 13%, indicating the
initiation and termination of the delamination process.
The Metcoloy 2q80Ni20Al coating arc sprayed in
air is bent to a strain of 11% after which the total
measured delamination length is 3 mm. Up to a strain
of approximately 6% the pattern is similar to that
recorded from the reference tube and Inconel 625 coat-
ing, Fig. 9b,c. Above a strain of 6% there is a stepwise
increase in energy level, which is interpreted as the
formation of cracks and a subsequent delamination. The
accumulated energy level does not deviate from the
reference tube and laser coating until a strain of 9.5%
is reached. The initial steeper rise in accumulated energy
in the strain interval 0.1–0.25% is due to equalisation
efforts made for adopting the curve to the Inconel 625
coating at higher strains.
The strains at which delamination is initiated as
interpreted from the acoustic emission measurements are
summarised in Fig. 10. The carbide containing HVOF-
coatings, Amperit 526 and Metco 3007, show the weak-
est adhesion strength and delamination is initiated at the
strains 1.0% and 0.9%, respectively. The performance
of the Metcoloy 2 coating deposited with the same
method is somewhat better and delamination is not
recorded for strains below 1.8%. The strains at which
delamination has been recorded for the same coating in
the arc sprayed condition are in the same range 1.4%
and 1.9% with air and nitrogen as carrier gases, respec-
tively. The effect of the 80Ni20Al addition to Metcoloy
2 is clearly seen from the fact that the delamination
strain increases to approximately 10% (columns 6 and
7), which reflects an increased adhesion strength. How-
ever, a small droplet size in the coating immediately
eliminates the positive effect as seen from columns 8
and 9.
215
Fig. 10. The strain at which delamination is initiated as determined
by acoustic emission. The number on the x-axis corresponds to the
one given in the legend denoting the coating materials.
3.4. Microstructural investigations
The microstructure of the Metcoloy 2 arc sprayed in
air and mixed with the 80Ni20Al bond coat was further
investigated due to the differences in adhesion strength
recorded. The splat size, which is the same as that
obtained with normal spraying parameters, is approxi-
mately 50 mm, Fig. 11a. Auger spectroscopy shows that
the only element present in the light areas which
originates from the 80Ni20Al bond coating material
(points 1, 3 and 5) is Ni. Al was not detected at all. In
an other study, it has been suggested that Al has
evaporated during the arc spraying process w11x. A more
significant net material loss than usual was also noted
during the coating production. The dark droplets origi-
nate from the Metcoloy 2 material (points 2, 4 and 6)
and Fe, Cr and Ni are recorded. Thus, Ni has diffused
into the Metcoloy 2 splats. Fig. 11b shows the same
material mixture as in Fig. 11a, but with a droplet size
of 200 mm. From Auger spectroscopy it is concluded
that a very limited intermixing between the Metcoloy 2
and 80Ni20Al phases has taken place in this case. Only
a minor concentration of Ni from the bond coat was
detected in the Metcoloy 2 phase, while Al evaporated
during the processing. On comparison image analysis
shows that the total splat boundary length is three times
smaller than for coatings built of small splats. In each
of the cases, the splat size was the same throughout the
coatings.
The Vickers hardnesses of the HVOF coatings Amper-
it 526, Metco 3007 and Metcoloy 2 are 800, 550 and
350, respectively. Arc spraying of Metcoloy 2 gives a
coating with Vickers hardness 320. Despite the differ-
ences, delamination is initiated at about the same strain.
Addition of 80Ni20Al into the Metcoloy 2 coating
results in a further hardness decrease to 220 HV for the
small splats quality and 150 HV for the large splats
quality.
216 ¨
A. Hjornhede, A. Nylund / Surface and Coatings Technology 184 (2004) 208–218
Fig. 11. Cross-sections of Metcoloy 2q80Ni20Al coatings (a) small splats (b) large splats (SEM microscopy).
4. Discussion
Adhesion tests have been performed on coatings,
deposited on low-alloyed steel tubes with the arc spray,
HVOF and laser techniques. Tensile tests only gave
delamination for the HVOF deposited coatings at a
tensile strength of 55–61 MPa, while the arc sprayed
coatings suffered from internal fracture at 38 MPa. The
laser coatings did not delaminate at all, but fractured in
the glue joint. The results obtained on the arc sprayed
coatings are in accordance with earlier ASTM 633 tests
w12x, which showed internal fracture on Metcoloy 2
coatings at stresses of 34"12 MPa. However, in the
same study HVOF deposited, Metco 3007 coatings
fractured in the glue joint at a stress of 69 MPa. The
discrepancy in the results is explained by the tube
geometry used in our study, where the surface curvature
induces additional peeling forces at the coatingyglue
interface.
Table 3
Correlation between delamination as determined by metallography and acoustic emission
Coating
Amperit 526, HVOF
Metco 3007, HVOF
Metcoloy 2, HVOF
Metcoloy 2, arc spray, air
Metcoloy 2, arc spray, N2
Metcoloy 2q80Ni20Al, arc
spray, air, large splats
Metcoloy 2q80Ni20Al, arc
spray, N2, large splats
80Ni20Al, arc spray, air, small splats
Metcoloyq80Ni20Al, arc spray, air
small splats
The traditional way of testing the degree of delami-
nation is tensile testing combined with optical micros-
copy. The method has the drawback that it requires
several experiments where coated tubes are bent to a
specific strain and then metallographically analysed in
order to determine any crack formation at the coatingy
substrate interface. Using acoustic emission makes it
possible to continuously monitor the crack initiation and
growth during delamination. Table 3 shows the correla-
tion between delamination as determined by metallo-
graphic analysis and the evaluation of acoustic emission.
For all coatings, the number of experiments where
delamination is detected by metallographic analysis is
noted. This is compared with the number of bending
tests where analysis of the acoustic emission has indi-
cated delamination on the same coating. Only two
samples both deposited with HVOF show a discrepancy
where delamination was detected by acoustic emission
analysis and not by optical microscopy. The explanation
Number of coatings which Number of coatings which
delaminated according to delaminated according to
metallography acoustic emission
0 1
2 3
3 3
7 7
3 3
2 2
2 2
3 3
3 3
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A. Hjornhede, A. Nylund / Surface and Coatings Technology 184 (2004) 208–218
may be in the sample preparation of the tested coatings.
During sectioning of the bent tube a 1.6-mm wide
material strip is cut away and thereby any delaminations
and cracks in this area have vanished. Further, large
stress concentrations and weak bonding in off-centre
areas of the coating can induce small cracks. These are
not detected during the metallographic analysis, which
is only performed along the centreline of the coating.
Contrary, the method of using acoustic emission records
all the deformation during the bending independent of
its location. However, the correlation between the two
methods is very good and the conclusion must therefore
be that acoustic emission is a suitable technique for
evaluation of coating adhesion.
In this study, arc sprayed coatings with small splats
and HVOF deposited coatings usually start to delaminate
in the strain interval 0.5–2.0%. Metallography revealed
that delamination is always accompanied by radial
cracks perpendicular to the coatingysubstrate interface.
When a radial crack has developed, the coating is
unloaded and the coatingysubstrate interface comes
under increased tension, resulting in crack growth and
delamination. In this region, a minimum of material
mixing takes place during thermal spraying and the
coating is thus bonded to the substrate surface by
mechanical interlocking w2x. The statement is supported
by the low adhesion strengths as measured with the
tensile test and the swiftness of the delamination process
after initiation. The laser coatings did not delaminate at
all, not even for strains up to 15%. The reason lies in
the laser process, where a small portion of the substrate
surface is melted and mixed with the coating material.
The result is a thin zone of metallic bonding w3x, which
strongly increases the adhesion strength compared with
the thermally deposited coatings.
Separate electrodes of Metcoloy 2 and the bond
coating material 80Ni20Al were arc sprayed into coat-
ings with two different splat sizes, ;50 mm and ;200
mm. The adhesion strength of the coating with the larger
splats is superior to that with the smaller ones. In fact,
addition of the bond coating material does not influence
on the adhesion strength at all, if the splat size is the
same as that for the pure Metcoloy 2 coatings. However,
the latter quality was only available with the smaller
splat size.
It has been shown w13x that the adhesion strength for
coatings made of Al and SUS308 steels arc sprayed in
air increases with the droplet size in the molten state.
The larger droplets impinging on the surface during the
spraying process have a higher kinetic energy. It has
been suggested that the impact introduces a peening
effect with accompanying compressive residual stresses
in the coating w13x. Thus, the adhesion strength of the
coating is increased. In the case of HVOF deposition,
the effect is larger due to the only partially melted
217
droplets where the smaller contact area results in a
higher impinging pressure w14x. However, the influence
of the coating microstructure was not taken into consid-
eration in any of the studies referred.
The present study shows that in the coatings com-
posed of large splats the splat boundary length is only
approximately 1y3 compared to the small size splat
coatings. Since the splat boundaries are enriched in
oxides and pores, their contribution to the weakening of
the coating is large and radial cracks are preferably
formed in these regions during tensile loading. Thereby
if the number of splat boundaries is minimised, the
radial cracking probability is reduced and the adhesion
strength improved.
Despite the large differences in hardness among the
coatings, delamination is initiated at about the same
strain. The coating hardness therefore seems to be of
minor importance for the delamination behaviour. The
hardnesses of the Metcoloy 2 coatings mixed with the
80Ni20Al bond coat are very low for both splat sizes.
In both cases, evaporation of Al during processing
creates an almost pure ductile Ni phase w11x. Thus, the
improvement in adhesion strength is due to the formation
of larger splats and not the presence of the bond coating
material.
5. Conclusions
The adhesion among coatings deposited on low-
alloyed steel tubes with arc spray (air or nitrogen as
carrier gas), HVOF and laser techniques was compared
with a modified four point bending test and acoustic
emission. The conclusions are as follows:
● Acoustic emission can be used for estimating the
strain at which coating delamination is initiated.
● The delamination is always initiated by the formation
of a radial crack.
● Coatings deposited with the laser technique show no
delamination for strains below 15%.
● Coatings deposited with HVOF start to delaminate
in the strain interval 0.8–1.8%.
● The adhesion strength of the arc sprayed coatings is
dependent on the splat size. Small splats give delam-
ination in the strain interval 1.4–1.9% while large
splats give delamination in the strain interval 10.5–
11.5%.
● Mixing a bond coating material into the arc sprayed
coating has no effect on the adhesion strength.
Acknowledgments
Financial support from the KME (Consortium for
Material Technology directed towards Thermal Energy
Processes) is gratefully acknowledged. Duroc AB and
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A. Hjornhede, A. Nylund / Surface and Coatings Technology 184 (2004) 208–218

Midroc Metalock are acknowledged for deposition of w8x X.Q. Ma, S. Cho, M. Takemoto, Acoustic emission source
¨
the coatings and Hoganas ¨ AB for provision of the analysis of plasma sprayed thermal barrier coatings during
four-point bend test, Surf. Coat. Technol. 139 (2001) 55–62.
powders. Finally, the tubes were supplied by Kvaerner ´
w9x Characterisation ´
par emission ´
acoustique de l’adherence et de
Pulping AB which is also acknowledged. ˆ
l’endommagement d’un revetement: ˆ
cas d’un revetement WC-
Co sur acier, D. Dalmas, S. Benmedakhene, C. Richard, A.
´
Laksimi, G. Beranger, ´
T. Gregorie, Comptes rendus de l’aca-
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