Tribology Infrrnafional Vol. 30, No. 7, pp. 491498.

1997
0 1997 Elsevier Science Ltd
All rights reserved. Printed in Great Britain
ELSEVIER 0301-679X/97/$17.00 + 0.00
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PII: SO301-679X(97)00012-1

re mode maps in the thin

scratch adhesion test

The scratch test has been used to assess thin coating adhesion
for some time now. In this test a diamond indenter is drawn
across the coated surface under an increasing load (either
stepwise or continuous) until at some load, termed the critical
load, L,, a well-defined failure event occurs; if this failure event
represents coating detachment then the critical load can be used
as a qualitative measure of coating-substrate adhesion. However,
it is well known that a range of possible failure modes can occur
and only some of these are dependent on adhesion. Other failure
modes which depend on plastic deformation and fracture within
the coating, rather than any adhesive failure at the coating
substrate interface, may be just as useful in the assessment of
coating quality particularly for tribological applications. In this
paper the load regimes in which the main adhesion-related failure
modes (spallation and buckling) occur as a function of coating
thickness will be presented for thermally grown oxide and
sputtered nitride coatings. The origin of the observed failure
modes and the use of the scratch test to assess coating/substrate
adhesion in a more quantitative fashion is discussed in the light
of these observations. 0 1997 Elsevier Science Ltd.

Introduction buckling failure modes result from interfacial detach-

The scratch test has been used to give a measure of
the adhesion of a range of coatings for some time now
-6. In the most common version of the test a diamond
stylus is drawn across the coated surface under an
increasing load until some well-defined failure occurs
at a load which is called the critical load, L,. If this
test is to be used to assess adhesion then this failure
must occur as a result of coating detachment which is
not always easy to identify.
The types of failure which are often observed in the
scratch test depend critically on the properties of both
substrate and coating. If the coating is very soft com-
pared to the substrate, considerable plastic deformation
will occur within it and the scratch test critical load
may be defined as the load at which the coating is
scraped off exposing the substrate 7. However, it is
not always easy to determine when this has occurred
and quantification of the failure mode is difficult. For
a hard coating on a softer substrate spallation and
Materiuls Division, Department oj. Mechanical,
facturivg Erzgineering, Herschel Building
Newcn~tle-llpon-T?irle NE1 7RlJ. UK
ment *x9 but a range of other cracks and deformed
regions can be observed. Both the spallation and buck-
ling failure modes are amenable to quantification and
are discussed in some detail in this paper. For hard
coatings on hard substrates the chipping observed in
the scratch test is almost identical to the lateral fracture
observed in the scratch testing of bulk ceramics. This
failure is occasionally observed to coincide with the
coating-substrate interface but this is not always the
case making the results of the test difficult to interpret.
Thus if scratch testing is to be used for adhesion
assessment only the spallation and buckling failure
modes are really useful. This generally limits the test
to the assessmentof hard coatings on softer substrates.
In this paper the scratch test failure modes observed
for hard coatings (sputtered TIN coatings and thermally
grown alumina oxide scales) are briefly reviewed. The
theoretical basis for analysing buckle and spa11failures
is introduced and some observations about failure
initiation and how the failure mode affects the locus
Materials and Manu- of failure will be made.
Universify of Newcastle,

Tribology International Volume 30 Number 7 1997 491

Thin film scratch adhesion test: S. J. Bull

Scratch test failure modes the same, which needs careful post facto inspection to
confirm in many cases.
The failure modes in the scratch testing of hard coat-
ings can broadly be split into three categories: If the scratch test is to be used for the assessment of
coating-substrate adhesion then it is the adhesion-
1. Through-thickness cracking (Fig l)-including ten- related failure modes which are most important. There
sile cracking behind the indenter .lO, conformal is a well-defined range of coating and substrate proper-
cracking as the coating is bent into the scratch ties where adhesion-related failures can be observed in
track ,I, and Hertzian cracking 8. the scratch test (Fig 3) and this restricts the range of
coating-substrate systems in which the test can be used
2. Spallation (Fig )-including compressive spall-
for adhesion assessment. In general it is most useful
ation ahead of the indenter ,l, buckling spallation
for hard coatings on soft or hard substrates where
ahead of the indenter or elastic recovery induced plastic deformation of the coating does not occur to
spallation behind the indenter 2 .
any great extent. However, there is a tendency for the
3. Chipping in the coating (akin to lateral cracking diamond stylus to wear during the test in cases where
in bulk ceramics). both substrate and coating are hard so the test has
been most widely applied to hard coating-soft substrate
systems. In such cases three main types of adhesion-
The type of failure which is observed for a given related failures are observed in the scratch test:
coating-substrate system depends on the test load, the
coating thickness, the residual stress in the coating and 1. Buckling-this failure mode is most common for
the properties of the substrate (e.g. hardness) as well thin coatings ( < 9 pm for an alumina oxide scale
as on test parameters such as indenter radius and on an iron-based alloy substrate, < 12 pm for TIN
sliding speed. Generally the critical load at which a on high speed steel). Failure occurs in response to
given failure mode first occurs, or occurs regularly the compressive stresses generated ahead of the
along the scratch track is used as a method of coating moving indenter [Fig 4(a)-(d)]. Localised regions
adhesion assessment. Comparisons between different containing interfacial defects allow the coating to
samples are only valid if the mechanism of failure is buckle in response to the stresses. Individual

(THROUGH-THICKNESS CRACKING

BRITTLE TENSILE CRACKING DUCTILE TENSILE CRACKING

HERTZ CRACKING CONFORMAL CRACKING

Fig. I Through-thickness cracking failure modes in the scratch test

492 Tribology International Volume 30 Number 7 1997

WEDGING/SPALLATION
Fig. 2 Intelfacial fuilure modes in the scratch test
Major Scratch Test Failure
1 lti0
/ Plastic Deformation
I/
Substrate Hardness
Fig. 3 Map of the main scratch test failure modes in
terms of substrate and coating hardness
buckles may then spread laterally by the propa-
gation of an interfacial crack. Spallation results
when through-thickness cracks form in regions of
high tensile stress within the coating [Fig 4(c)].
The presence of plastically piled-up material ahead
Or the indenter can enhance this failure mode.
Cnce the buckle has occurred the scratch stylus
passes over the failed region crushing the coating
Thin film scratch adhesion test: S. J. Bull
/INTERFACIAL FAILURE 1
BUCKLE SPALLATION
RECOVERY SPALLATION
into the surface of the scratch track formed in the
Regimes
substrate. At this time there may be enhanced
coating removal or the failure can disappear com-
pletely depending on its size and the toughness of
the coating. Buckling failures typically appear as
curved cracks extending to the edges of or beyond
the scratch track. Regions of spallation associated
with buckle failures have edges perpendicular to
the coating-substrate interface.
2. Wedge spallation. Once a critical coating thickness
is achieved the coating becomes too stiff to buckle
and reduce the stresses ahead of the indenter.
\I
Compressive shear cracks now form through the
1 ,
thickness of the coating before interfacial failure
is observed [Fig 4(e)-(h)]. These cracks have slop-
ing sides [Fig 4(f)] and the continued forward
motion of the stylus drives wedges of adjacent
coating under the segment bounded by the shear
crack causing decohesion of the interface. Large
enough displacements will cause a region ahead
of the indenter to spall. In extreme cases the
scratch diamond can drop into the hole left by
removal of the coating and there is a dramatic
increase in scratch width and scratch depth.
3. Recovery spallation-this failure mode is associa-
ted with the elastic recovery which occurs behind
the stylus as it travels over the coated surface and
depends on plastic deformation in the substrate and
Tribology International Volume 30 Number 7 1997 493
Thin film scratch adhesion test: S. J. Bull
Coating
Increasing applied
stress
zone of athermal
damage
Fig. 4 Schematic of the main stages in adhesion-related coating failure
(h) wedging
through-thickness cracking in the coating. After the
stylus passesand the scratched region is unloaded
the elastic deformation jn the coating-substrate
system is relaxed. However, due to the plastic
deformation in the substrate, which results in the
formation of the scratch track, it is not possible
to completely relax the substrate elastic defor-
mation and a residual stress remains. If through
thickness cracking has occurred in the coating
any residual strain on it can be more completely
relaxed-tensile recovery stresses in the coating
are converted into shear stresses at the coating-
substrate interface near to these cracks. The propa-
gation of interfacial shear cracks due to these
stresses can lead to spallation either side of the
scratch track. This failure mode is not generally
observed for hard coatings on soft substrates where
the adhesion is good and will not be discussed
further in this paper.
The buckling and spallation failures which are observed
for TiN coating and alumina oxide scales are discussed
in some detail in the following sections.
Experimental
Samples of stainless steel (304) and the oxide disper-
sion strengthened alloy MA956 were cut into 20 x 10
x 2 mm sections, polished to a 1 mm diamond finish
and cleaned and degreased prior to use. The 304
stainless steel coupons were coated with TIN by sputter
ion plating I2 at a temperature of 500C and a bias
voltage of - 35 V. Thicknesses in the range 1-15 pm
were deposited and measured by ball cratering. Prior
to TIN deposition and samples were sputter cleaned
494 Tribology International Volume 30 Number 7 1997
in Compression
areas of
decohesion
directions
of crack
propagation e-
sites of
tensile
interface
mechanisms, (n)-(d) buckling and (e)-
and a 120 nm titanium interlayer was deposited to
promote adhesion. The MA956 samples were weighed
and placed in alumina crucibles prior to isothermal
oxidation in flowing laboratory air at 1150C and
1250C for times up to 1400 h. This produces oxide
scale thicknesses up to 20 pm. Both samples and cru-
cibles were weighed before and after exposure to pro-
vide an estimate of scale thickness and the amount of
spallation. It was confirmed that a weight gain of
1 mg/cm equates to a scale thickness of around 5 pm
l3 by ball cratering.
Scratch testing was performed using a CSEM manual
scratch tester fitted with a Rockwell C diamond (120
cone with a 200 pm radius hemispherical tip). This is
a dead-loaded machine where a separate scratch is
made for each applied load. A scratch length of 3 mm
was used and loads were applied from 200 g upwards
in 200 g increments. The tester is fitted with acoustic
emission monitoring equipment which can detect emis-
sion in the vicinity of 100 kHz which was used as an
on-line failure monitor. Buckle failures lead to a small
increase in acoustic emission whereas wedge spallation
leads to a much more dramatic increase. However,
although acoustic emission can given an indication of
failure mode, careful reflected light microscopy exam-
ination was necessary to confirm this and determine
the critical load.
In this sort of scratch test, care has to be taken in
setting the critical load criterion since it is known that
there is a distribution of flaws at the coating/substrate
interface 6. In this study the load at which failures are
first observed to occur regularly along the scratch track,
correlating with an increase in acoustic emission, was
used to avoid problems with isolated defects dominat-
ing the results. The failure mode is somewhat subjec-
 Thin film scratch adhesion test: S. .I. Bull

tive, but since the total number of wedge spallation Sputter Ion Plated TiN
failures was low, a full Weibull statistics analysis, as
detailed in 6, was not possible.

Results

Failure modes
For both TIN and alumina scales two types of scratch
test failure modes related to adhesion were observed
(Fig 5). For thjn TIN coatings buckling failures were
observed within the track [Fig 5(a)] but these extended
outside the track for the thin oxide scales on MA956
[Fig 5(c)]. For thicker coatings, wedging failures were
observed [Fig 5(b) and (d)]. The wedge is most appar-
ent at the front of the spalled region where the com-
pressive stresses on the coating are greatest. The sides 0 2 4 6 8 IO 12 14
!
16
and rear of the spalls are delineated by through-thick- Thickness (pm)
ness cracking which is less obviously wedge-like. For
the TIN coatings the transition to wedging spallation Fig. 6 Variation of the critical load for coating detach
occur! at a slightly greater thickness than for the oxide ment in the scratch test with coating thickness for
scale on MA956 (Figs 6 and 7).
sputter ion plated TiN on stainless steel

Failure load regimes and stresses

MA956
For all coatings investigated the critical load for buckle 4Qxl
formation increases as the coating thickness increases
(e.g. Figs 6 and 7). Wedging spallation does not occur 3500
until higher coating thicknesses and the critical load
for wedging failure decreases as the coating thicknesses 3ooo
increases. In some cases (e.g. near the wedge/buckle
transiGon) it is possible to see both types of failure 2500
mode on the same scratch track, but generally only
one type of failure is observed. 2ooo

The ,;tresses responsible for coating detachment, cr,,

are a combination of the residual stress remaining in 1500

the coating at room temperature, crR, and the stresses

introduced by the scratch stylus, cs. Thus IOIYJ

500

a, can be measured for both TIN coatings and the

oxide scales on MA956 by X-ray diffraction using Thickness (urn)

Fig. 7 Vuriation of the critical load for coating detach-

FeCrAI and FeCrAlY: 1100C Oxidation ment in the scratch test with scale thickness for an
alumina oxide scale grown on MA956 at 1250C and
1150C

the well-known sin $ method I. Table 1 tabulates

measurements made in this study. The technique is
most applicable to the thickest coatings due to the X-
ray penetration depth which is greater than the coating
thickness in all cases. No significant variation in
500
residual stress as a function of coating thickness was
observed in the films tested here.
0 However, it is much more difficult to determine the
0 2 4 6 8 stresses introduced by the scratch diamond, us. No
Thickness (pm) adequate theoretical model exists to predict the stresses
generated ahead of a moving indenter in a bulk elastic-
Fig. 5 Scanning electron micrographs of scratch test plastic material, let alone in a coated system 15. It is
failure modes in TiN coatings: (a) buckling and (b) necessary to estimate the stressesusing other methods.
wedge spallation; and alumina oxide scales on MA9.56: In the scratch testing of TIN coatings on stainless steel
(c) buckling and (d) wedge spallation or other steel substrates it has been shown that the
Tribology International Volume 30 Number 7 1997 495
Thin film scratch adhesion test: S. J. Bull

Table 1 Residual stress at room temperature in

the coatings determined by X-ray diffraction (sin2
$ method)

Coating-substrate system Compressive

residual stress
(GPa)

5 pm TIN on stainless steel 6.03 i 0.07 --e MA956 Buckle

-- MA956 Spa11
7 pm TiN on stainless steel 6.15 f 0.14
5 pm Al,03 scale on MA956
Formed at 1250C 3.91 f 0.09
Formed at 1150C 3.69 + 0.10

10

critical load for coating detachment is reduced as the Thickness (Nm)

residual stress in the coating increases 16. In this case

the residual stress is changed by using different levels Fig. 8 Varintiorz of the compressive stress to initiate
of ion bombardment (bias voltages) during deposition failure in the scratch test with coating thickness ,for
and can be measured by X-ray diffraction. Equating TiN coatings and aluminn scales or1 MA956 grown
the change in critical load measured in the scratch test nt 1250C
on fully dense TIN coatings with the difference in
residual stress measured allows a calibration factor to
be determined. In the case of the TIN films tested Table2 Properties of TIN and alumina coatings
here: 1 g in the scratch test is equivalent to a 0.6 MPa used in the calculations
compressive stress ahead of the indenter.
Material Youngs Poissons ratio
For MA956 oxidation experiments carried out at modulus (GP)
1150C and 1250C produce alumina scales with a
difference in residual stress of 224 MPa (Table 1).
Scratch testing these scales (Fig 7) shows a difference &OS 380 0.26
TiN 600 0.21
in failure load of 590 g for wedge spallation failures
(i.e. I g is equivalent to 0.38 MPa). The scales pro- Measured from phonon dispersion curves on bulk materials-
duced by oxidation at 1150C require a higher scratch values measured from scales or coatings by other techniques
test load to produce failure than the scales produced are often lower
by oxidation at 1250C as expected from their lower
residual thermal stress. There is no significant differ-
ence in failure load for the two test temperatures for and is plotted against the measured width of the scratch
the buckle failures which implies that the residual stress track in Fig 9 for both TiN and MA956. The corre-
on the coating is much less important in this case. lation between the track width and the size of the
defect responsible for buckling is very good. Changing
Using the two calibration factors the failure
stress/thickness behaviour for the two materials is
shown in Fig 8. Considerably higher failure stresses
are observed for the TiN coatings which are known to
be very adherent.

Discussion
Much of the theoretical background for modelling of
buckling and spallation failure modes has been
developed for oxide scales under conditions of ther-
mally induced stresses. According to Evans I7 the
critical buckling stress a, is given by

where E, and u, are the Youngs Modulus and Pois- 10 20 30 40 50 60 70 80 90

sons ratio of the coating, f the coating thickness and R
the radius of the circular area of interfacial detachment Calculated buckle radius (pm)

necessary to cause buckling. This predicts that the

critical buckling stress should increase with coating Fig. 9 Plots of calculated interjbciul defect radius
thickness as is observed here. Using Equation (2) and against scratch truck width for TN contirzgs on stain-
the data in Fig 8 and Table 2, R can be calculated less steel and alumina scales on MA956
496 Tribology International Volume 30 Number 7 1997
 Thin film scratch adhesion test: S. J. Bull

the Youngs Modulus of the coating, which might be 8.6

necessary to take into account the fact that the proper-
ties of scales and coatings are not the same as those
of bulk materials, will alter the size of R but does not
affect the relationship with the track width. It is thus
likely that the plastic deformation in the substrate,
which defines the scratch width at the failure loads
observed here, is responsible for the initiation of buck-
ling. in the region below the coating the constraint 7.8
from the harder coating on the deformation of the
softer substrate leads to the generation of high shear 7.6
stresses and the propagation of an interfacial shear
crack. It is this shear crack which provides the initial
disbond which causes buckling. Since plastic defor-
mation in the substrate is necessary to form the buckle-
initiating defect this explains the well-known obser- 250 260 270 280 290 300 310 320 330
vatior: that the critical load for coating detachment UP (dR)
increases as the substrate hardness increases and the
size of the scratch track at a given load is reduced Is.
The wedge spallation failure mode depends on two
distinct processes occurring 17. Firstly a compressive
shear crack must form in the coating and then interfa-
cial detachment occurs. According to Evans I7 the
biaxial stress necessary to cause the wedge crack, uW,
is given by

(3)

where y is the fracture energy and A the width of the

wedge spalled region. This is independent of the thick-
ness of the coating. The biaxial stress to produce the
spall, o,,, after shear cracking has occurred is given by

(41 200 220 240 260 280 300 320 340

where 3/~ is the interfacial fracture energy. The total

failure stress is given by the sum of these two.
Fig. 10 Variation of failure stress with Id for (a) TiN
Clearly by plotting the measured failure stress, aF, coatings on stainless steel and (b) alumina scales
against the reciprocal of the square root of coating on MA956
thickness, the two contributions can be separated. This
is shown in Fig 10 for the two types of coating. Table
3 gives values for yF and (T, for TIN and MA956. In Table 3 Compressive failure stress and intetfacial
fact :he biaxial stress assumption, whilst valid for the fracture energy for TIN and MA956 determined
thermal and growth stresses,is not strictly valid for the from wedge spallation failures
scratch induced stresses which are closer to uniaxial.
How-ver, in both cases investigated here the scratch Substrate- Interfacial Failure stress,
induced stresses are much smaller than the biaxial coating fracture energy, u, (GPa)
therr_lal and growth stresses so this is a reasonable yF (J/m*)
first approximation.
MA956/AI,O, 28 3.72
The interfacial fracture energy for MA956/alumina is
304rTiN 451 2.52
reasonably low and represents predominantly brittle
failure with little crack tip plasticity. In fact the
Average value-the interfacial fracture energy varies with
observed value is similar to that determined for bulk oxidation temperature.
alurrina from fracture toughness tests ( - 20 J/m 19)
but is higher than values calculated for alumina scales
frorr tensile test data. For instance, Schutze 2o quotes materials (e.g. microcracking ahead of the crack tip)
values of scale fracture toughness between 0.4 and which are not active in the scales where the measured
1.3 MPam* which give fracture energies between 0.2 values are close to the surface energy of the material
and 2.2 J/m using yF = KlC2/2E. The discrepancy as expected. Careful microscopy shows that the failure
between the measured values for scales and bulk cer- crack propagates at or close to the interface for MA956
amics probably arises due to the existence of other wedge spallation so some crack-tip plasticity is prob-
crack energy absorption mechanisms in the bulk ably occurring.
Tribology International Volume 30 Number 7 1997 497
Thin film scratch adhesion test: S. J. Bull

The much higher interfacial fracture energy for TIN is plastic deformation immediately below the coating.
representative of more ductile failure where more blunt- This means that hard, ductile substrates are preferred.
ing of the crack tip can occur by plasticity. The failure To reduce the susceptibility of the coating-substrate
crack appears to propagate along the interface in this system to wedge spallation increasing the toughness of
case since the fracture energy is between that expected the coating to prevent shear crack propagation and
for TIN and the substrate. This is confirmed by ensuring that interfacial crack propagation actually
microscopy - it is not possible to detect any TIN at occurs in a ductile fashion is required.
the bottom of wedge spalls, nor any substrate material
To derive maximum benefit from the scratch test better
attached to spalled debris by X-ray analysis in the
theoretical models for the stress fields generated by
scanning electron microscope.
the moving indenter in coating-substrate systems are
The measured fracture stress for alumina on MA956 required.
is close to the residual stress in the coating measured
by X-ray diffraction showing that spontaneous shear
Acknowledgements
cracking probably occurs on cooling but at low tem-
peratures. Wedge spallation has been observed to occur This work was supported by the Corporate Research
on cooling alumina scales by 1070C on MA956 pre- Programme of AEA Technology and builds on results
viously 2. This temperature drop generates to a com- obtained under BRITE/EURAM contract BE7972 on
pressive thermal stress of - 3.9 GPa in the absence of How to improve the failure resistance of alumina
creep which is reduced to 3.7 GPa when high tempera- scales on high temperature materials.
ture creep is allowed to relax some of the substrate
stresses.The fact that failure occurs at a low tempera-
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498 Tribology International Volume 30 Number 7 1997