ELSEVIER Thin Solid Films 286 (1996) I I 1-121 ~~,e..

Investigation of the stresses and stress intensity factors responsible for

fracture of thin protective films during ultra-micro indentation tests with
spherical indenters
E. Weppelmann a,l, M.V. Swain b,~
Fraunhofer-lnstimte for Material Mechanics, Wi~hlerstr. ! i, 79108 Freiburg, Germany
h Division of Applied Physics, Commonwealth Scientific and Industrial Research Organization, Lindfield, NSW 2070, Austra'ia
Department of Mechanical and Mechatrtmic Engb~eering, University of Sydney, Sydney, NSW 2006, Australia
Received ! l August 1995; accepted I I December 1995

Abstract

This paper reports on the mechanical characterization of thin hard films deposited on softer substrates using the micro-indentation technique
together with spherically tipped indenters. Alt,~r a short review of the deformation and fracture behavior the indentation process is simulated
using a finite element analysis in order to determine the stresses responsible for the first fracture event of the film. A fracture mechanics
analysis is presented that uses the weight function method to calculate the stress intensity factors K~and K, within the near surface region of
*"," film. A fracture criterion, for multiaxial loading conditions is used to calculate the stress intensity factor Kt ~pp~.It will be shown that for
ms which are thin compared to the radius of the indenter first fracture should occur under a Mode-1 loading condition. For the cases where
the film was thick compared to the indenter radius mixed mode loading conditions prevail and the resultant fracture path is dependent on the
nature of the film microstructure.

Keywords: Stress; Thin flints; Physical vapour deposition (PVD)

1. Introduction Recently, Sw'.tin and coworkers 112-141 introduced the

use of spherically tipped diamond indenters into the micro-
In thin film technologies hard protective coatings are indentation technique to study the deformation and fracture
becoming more and more important. There is thus an increas- behavior of thin hard coatings deposited on softer substrates
ing need for the mechanical characterization of such layered by physical vapor deposition (PVD) techniques. They
systems. A simple method for this purpose is the micro- showed that, with spherical indenters, one is able to monitor
indentation test. In this test, a diamond indenter is pushed the occurrence of the first and subsequent circumferential
into the surface of a sample under continuous measurement cracks through the films. In their studies they were able to
of the applied load and the resulting penetration depth. Until describe the crack path through the coatings using scanning
now, experiments to determine the mechanical properties of electron microscopy (SEM) observations of cross-sections
thin protective layers with the micro-indentation technique of the indented regions.
have been carried out in most cases with Berkovich and Vick- After a shc~rt review of the deformation and fracture a finite
ers indenters (three- and four-sided diamond pyramids). The element analysis of the indentation process is presented in
common properties which were measured with these indent-
this study in order to generally describe the stresses respon-
ers are the hardness and the elastic modulus of thin films [ 1-
sible for crack initiation and crack propagation. Furthermore,
4]. Some workers also reported about the occurrence of
a simple fracture mechanics analysis rrethod will be pre-
cracks through the film (radial and circumferential) and
sented to calculate the stress intensity factors along the initial
about interfacial failure during micro-indentation tests with
crack path.
pointed indenters [5-11]. Methods for a first estimation of
An early finite element study of an elastic contact between
the fracture toughness of the film and the interface were also
a rigid sphere and a flat infinite half space of glass protected
presented by some of these workers 18-11 ].
by a thin elastic layer was presented by van der Zwaag and
' Present address: Kanonierstrale 20, 76 ! 85 Karlsruhe, Germany. Field [ 151. They described the influence of the elastic film
0040-6090/96/$15.00 © 1996 Elsevier Science S.A. All rights reserved
SSD10040-6090 ( 95 ) 08525-4
 112 E. Weppelmatm, lt4.V. Swain / Thin Soli,t Films 286 ¢! 996) 1 i 1-121

on the stress situation in the glass substrate varying the mate- in three stages (see Fig. 1). In the beginning of the loading
rial parameters and the thickness of the fihn. They found that process the deformation will be entirely elastic and reversible
the maximum radial tensile stress in the glass surface can be (stage 1). Upon further loading the stresses in the substrate
reduced by an elastic protective layer. However, this effect reach the yield point and irreversible plastic deformation
is accompanied by an increase in the maximum radial tensile starts to occur (stage 2). Eventually, the stresses in the film
stress in the surface of the protective film itself. accumulate up to the point where the stress intensity factor
More recently, Djabella and Arnell [ 16,17] presented an of a critical intrinsic flaw equals the fracture toughness of the
extensive finite element study of the general stress situation film and first fracture occurs (stage 3). Further increasing the
in an elastic contact on mono- and double-layered coating load Ktay then lead to subsequent fracture events in the film.
systems. Their finite element model of the layered sample In order to confirm this behavior, further indentation meas-
was loaded with pressure distributions identical to those aris- urements were carried out by the authors on TiN films (PVD)
ing during Hertzian indentation of a homogeneous elastic deposited on tool steel as well as on TiAIN films (PVD) on
half-space by spherical and cylindrical indenters. They also stainless steel. Again, first and subsequent steps could be
studied the influence of the elastic modulus and the thickness observed on the load--displacement data of indentation tests
of the coatings on the stress field generated by the Hertzian which were loaded beyond the onset of fracture. SEM cross-
pressure field. Although these studies give a good qualitative sectional observations of the indented regions could not be
idea of the general stress field of an elastic contact situation produced from these samples. Therefore, the crack path
between a sphere and a layered sample there is still the need through these films could not be clarified. Nevertheless, the
for a more realistic simulation of the indentation process. similarity of the crystal structure between the films on steel
In this study, the process of spherical indentation on a thin and the TiN films on silicon suggest, that the crack path
elastic mono-layer on a softer substrate will be simulated should be independent of the substrate material and similar
using the finite element analysis technique. In this simulation to the fracture behavior previously described with cracks
the indenter will also be modeled by an element mesh in order following the grain boundaries. Obviously these films were
to account for the deformation of the indenter. For both, the better adhered onto their steel substrates because there was
indenter (diamond) and '.he film (TIN) only elastic defor-
no indication for lateral cracks.
mations will be allowed whereas plastic deformation will be
allowed for the substrate material (stainless steel). This paper (1)
rel~orts on the influence of the film thickness on the stresses
which are responsible tbr the break through events of the n IP
film.

V
2. Deformation and fracture behavior
(2) p ,~
Hard protective coatings deposited by a physical vapor
deposition technique (PVD) on sorer suhstratcs in many
cases consist of ~ columnar grain structure, In such films the
axes of the elongated grains are perpendicular to the film
surface. Due to this specific grain structure it is obvious that
a crack, starting from a pre-existing flaw in the surface, will
proceed along the grain boundaries, i.e. along lines vertical
to the surface. As mentioned above, Swain and coworkers
[ 12-14] described the deformation and fracture behavior of (3) R IP
such films during spherical indentation tests. Studying the
h
behavior of Till films on silicon, they were able to identify
the occurrence of the first and of subsequent circumferential
cracks by sign:ficant steps on the loading cycle of the load-
displacement carve, Using SEM cross-sectional observations
through the indented regions they showed clear evidence that
the TiN films were indeed broken along their grain boundaries
tic region
vertical to the surface. Long lateral cracks along the film-
substrate interface were also visible on these SEM observa- Fig. 1. Principle oftbe deformation process during spherical indentation on
tions indicating delamination of the film. brittle films deposited on elastic-plastic behaving substrates. (a) Completely
Following their studies, the deformation process during elastic and reversible deformation in the beginning of the indentation proc-
spherical indentation tests on brittle protective layers depos- ess. (b) Plastic deformation in the substrate during further loading. (c) First
andsubsequentfray;turnwhen the stress intensity factor of an intrinsic flaw
ited on elastic-plastic behaving substrates can be described exceedsthe fracturetoughnessof the film.
 E. Weppelmann, M. V Swain / Thhz Solid Fihns 286 (1996) 111-121 113

Fig. 2 shows an example of a typical load-displacement ual stresses in the film, the constitution of the film-substrate
curve measured on a 3.5 ~m thick TiAIN film on stainless interface, the film thickness and the surface roughness of the
steel using a nominally 20 I~m radius indenter. A calibration film.
of the geometry of this indenter revealed that he had a 35 t~m Whether steps occur during the loading cycle of an inden-
radius area at the first tip region where contact was expected. t~,tion test or not strongly depends on the ratio of R/t, where
Two steps are visible on the loading cycle of the curve indi- R is the radius of the indenter and t the thickness of the film.
cating the fracture events. This figure also shows a divergence For large values of R / t the energy released due to the break-
from the elastic response (where hot p2/3) at loads in excess through event in itself may be too small compared to the
of = 120 mN suggesting plastic deformation of the underly- energy necessary to produce a significant advance in the
ing substrate. A SEM micrograph of the indented region is deformation of the indented region, resulting in a sudden
shown in Fig. 3. Two circumferential cracks can be observed increase in depth. In those cases the substrate material will
which correspond to the steps on the load-displacement curve dominate the deformation behavior of the indentation. For
in Fig. 2. very small values of RIt the influence of the substrate van-
What makes this behavior interesting is that the first break- ishes and the situation becomes similar to the case of the
through events, indicated by the first step on the load--dis- indenter penetrating an infinite half-space consisting of the
placeme.at data, usually occur at a critical load which is film material only. In those cases, whether fracture can be
characteristic for a specific sample configuration and testing monitored by significant steps on the loading cycle of an
geometry. Therefore, using the micro-indentation technique indentation test or not will depend on the amount of elastic
with spherical indenters, it is possible to measure a critical strain energy that can be accumulated in the sample material
load for the first crack in a thin elastic layer deposited on a prior to fracture. Therefore, when investigating the fracture
soft substrate. Of course, such a critical load depends on the behavior of thin films it is necessary to adjust the radius of
radius of the indenter and on the constitution of a coated the indenter to the thickness of the coating in order to be able
sample. The sample parameters that influence such a critical to detect the first onset of fracture.
load for fracture are the material properties of the film and Having the deformation and fracture behavior described a
substrate, the composition and structure of the film, the resid- fracture mechanical analysis can be carried out to estimate
the fracture toughness of the coatings. For an analysis of the
400 /Elastic , ~g first break-through event the stresses along the predicted
I P [toNI / .." ... crack path have to be calculated. Because of the lack of
j1 =l analytical solutions for such elastic-plastic contact problems
---/
~'UU l
/ Plast, response t"
ofsu~otrate"'-,~_.
•
°°""
L" " , , . "
¢,~-~ ~
" "7""
Film
===
/
.1"
J
#
/
the indentation process has to be simulated using a linite
,,,,, tr,cture/ element analysis techninue in order to determine the stresses
responsible for fracture.

°o 3~T- ....... 6oo 9oo

Fig. 2. l~,ntd-dJsphlcenl~r,i cnrve of il spherical indenttition test on n 3.5 it,lit 3. The analysis model
thick TtAIN film doposli,~d on stainless steel using a 35 I~ln radiused indente,'.
The loading cycle exhibits two major steps indicating two fracture events.
The ABAQUS code was used for the axisymmetrical finite
element analysis of the contact problem. Because ot the sym-
metry of the contact situation only half of the indenter and
the sample were modeled using a two-dimensio~al mesh
together with axisymmetrical elements (see Fig. 4). The size
of the model was chosen large enough compared to ~he con-
tact dimensions in order to ensure that only minimal boundary
effects contribute to the stress analysis (A/a = B/o > 100).
The contact between the surface of the indenter and the spec-
imen was modeled with special contact elements. These ele-
ments allowed a sliding movement between the two surfaces.
Furthermore, the contact was modeled without the c~ntribu-
tion of friction, assuming that friction does not affect the
stresses within the indented region. The indenter was loaded
along its upper side which was allowed to shift only parallel
to itself along the axis of symmetry. The contact area was
Fig. 3. SEM picture of an indentation in a 3.5 p,m thick TiAIN film deposited designed so that a minimum of 50 nodes was in contact on
on stainless steel carded out with a 35 Ixm radiused indenter. Two circum-
each surface after the maximum load was applied. Around
ferential cracks within the contact area correlate well with the steps on the
loading cycle of the load-displacement curve shown in Fig. 2. the area where the edge of contact could be expected, the
114 E. Weppelmann, M. E Swain / Thin Solid Fihns 286 (1996) ! ! i-121

P by using a constant radius of the indenter and varying only

the thickness of the film. Of course, if a constant maximum
load would be used in each of these cases the gradient of
deformation would differ from very deep indentations on the
detail / thinnest film to very shallow indentations on the thickes."film.
In order to produce similar deformation gradients the load
was adjusted that a constant value of the ratio R/h was
..... tI reached, where h is the depth of penetration of the indenter
into the specimen surface. In this study a value of 20 was
iz
chosen for the ratio of R/h.
B
14

~ ~,\\NN\\NN\\\NN".,'~ N\\\\\\\\\'¢.
Fig. 4. The axisymmetrical model used for the finite element analysis of the 4. The stresses responsible for fracture
indentation process.The elastically modeledindenter was loadedon its upper
side v ~,icb was allowed to shift parallel to itself along the axis of symmetry.
4.1. R/t= 20 /R/a=4.1, a/t=4.9]
mesh was further refined in order to resolve higher stress
gradients. The results of the finite element analysis of the spherical
In the finite element model the material properties of dia- indentation test on the thinnest coating studied are shown in
mond, TiN and stainless steel were attributed to the indenter, Fig. 5(a)-5(d). A plot of the load P on the indenter versus
the film and the substrate respectively. The elastic material the actual penetration depth h into the sample is shown in
parameters were: for the indenter, E~= 1050 OPa, v, =0.15; Fig. 5 (a). Because of the effect of geometric similarity both
for the film, El=480 GPa, vt-=0.2; and for the substrate, the load and the penetration depth have been made dimen-
Es = 210 GPa, vs=0.3; where E corresponds to the elastic sionless by division with their maximum values Pro=, and
modulus and to Poisson's ratio. To allow plastic deformation h,,=, respectively. It can be seen on this load--displacement
in the substrate material a bilinear stress-strain curve of a curve that the deformation behavior is dominated by the plas-
stainless steel was chosen with Rc.~= 600 MPa for the yield ticity of the substrate material.
strength and Rm= 900 MPa for the tensile strength at a plastic Fig. 5(b) shows the radial stress in the film surface plotted
strain of %t =0,04. The film was modeled without the con- against the ratio of r/a, where a means the radius of the circle
tribution of residual stresses. of contact and r is a coordinate directed radially outward
Four values of the ratio of R/t have been chosen in this starting from the axis of symmetry. The radial stress was
study, namely 20, 6.7, 2 and 0.67. These ratios were obtained found to be compressive within tile area of contact, whereas

2°i
lO

ol
~mml;ea~m= ~ . -_-_:.

/ ~ hmax -I0 rla

0 (a) I 0(Io) 1 :Z 3

20
"-.~.rr [GPa] .... rla = 1,oo 1;rz [GPa]
~':"..~.~'. ~ ...... rla = 1,08
~ ~ ~ . --- rla = 1 24

"'""':: ............................. . ..

. . . . r/a = 1 , 0 ~ - . " . . " . . \

z/t ...... rla = 1112 Z / t --'ix.'i~
-20 i

0 (e) 1 0 (d) 1
Fig. 5. Results of the finite element simulation for R h = 20. (a) The simulated load-displacement curve. (b) Curve of the radial stress along the surface. (c)
Curves of the radial stress along vertical lines through the film at different locations rla. (d) Curves of the shear stress through the film.
 E. Weppelmann, M. V. Swain/Thin Solid Films 286 {1996) 111-121 i 15

high radial tensile stresses occurred outside the contact zone 4.2. R/t=6.7 [R/a =5.3, a/t= 1.3]
with a maximum tensile stress at r/a = 1.24.
To investigate the stresses which could be responsible for Fig. 6 ( a ) - 6 ( d ) shows the results obtained on the film that
the initiation and propagation of circumferential cracks stress was modeled three times thicker as the coating described
curves along lines through the film vertical to the film surface previously. The load--displacement curve in Fig. 6(a) shows
were determined. The lines were placed at different locations that the deformation process is still severely influenced by
outside the circle of contact, i,e. at values of r/a > 1. The the plastic deformation of the substrate material. The radial
radial and shear stresses through the film are shown in Fig. tensile stress along the film surface reaches its maximum
5(c) and 5(d). The stresses are plotted against z/t, where t value far outside of the area of contact at r/a = 2.04 (Fig.
means the film thickness and z is a coordinate vertical through 6(b)).
The curves of the radial stresses through the film shown in
the film starting from the surface. Thus z / t - 0 corresponds
Fig. 6(e) differ from the stress situation described previously
to the surface of the film whereas z/t = 1 is equivalent to the
for the thinner film. Following the line located closest to the
film-substrate interface.
edge of contact at r/a-- 1.07 the radial stress is first com-
As can be seen in these diagrams, the radial tensile stresses
pressive near the surface but becomes tensile near the inter-
are biggest at the surface with a maximum value at r/a = 1.24.
face. This behavior changes gradually toward the location
They decrease with increasing depth but do not become com-
where the maximum radial tensile stress is reached at r~
pressive until the depth exceeds 60% of the film thickness,
a = 2.04. There the radial tensile stress decreases from its
i.e. z/t 0.6. The greatest shear stresses occur within the coat- maximum value at the surface until it becomes compressive
ing at around z/t 0.4 but they are a magnitude smaller than at a depth of z/t = 0.53.
the radial tensile stresses. Within the interesting region, the The shear stresses shown in Fig. 6(d) again reach their
maximum shear stress was found under the edge of contact greatest values in the middle of the film at z/t 0.5 with the
at r/a = 1 ,~,~dz/t = 0.42. maximum value close to the edge of contact at r/a = 1.07.
This stress situation suggests that a circumferential crack The magnitude of the shear stresses is about the same as the
is likely to initiate and propagate through the film mainly due magnitude of the radial tensile stresses.
to the maximum radial tensile s',resses at a small region If an uniform distribution of small pre-existing flaws in the
around rla = 1.24 outside the edge of contact. It can also be surface of the film can be assumed, the most likely location
assumed that the shear stresses play a minor role in the frac- for the initiation of a crack will be at r/a = 2.04 where the
ture process because of their smaller maximum value which radial tensile stress reaches its maximum values. Only if a
is furthermore located exactly at the edge of contact where large pre-existing flaw is located near the edge of contact
only small radial lensile stresses occur. might a crack be initiated by a mixed mode stress situation

101
Grr[GPa]
01
=
I
-10
/
-20 /
-30 J r/a
4
00 (a) 1 0(b)

~r/a = 1,07
.... e r r [ G P a ] - - - rJa = 1,07 1;rz [ G P a ] ~ / ~ . ~ . . ~ _ _ _ rta = 1,22
"'.... . . . . r/a = 1,22
. . . . . - " - rla = 1,43 ..~

Z:;i: : :" . .............. -':::i::\

""- """ : ..... r/a = 2,04 """ '"'...~ ~" .. , .
:,::;2;2 ...............
. . . . . . . . . . . .

~r/a=3,26 z/t
J
""t ............ z / t .............. ".::
-9
0 (c) 1 0 (d) 1
Fig. 6. Resultsof the finite elementsimulation for R/t = 6.7. (a) The simulatedload-displacementcurve. (b) Curveel' the radial stress ,'gong the surface. (c)
Curves of the radial stress along vertical lines through the filmat differentlocations r/a. (d) Curvesoft~.~s:,earstress through the film.
 116 E. Weppelmann,114,V, Swain/ ThinSolid Films286 (1996) 111-121

consisting of a radial tensile stress and shear stress. Another be found directly under the edge of contact but is shifted
possible location for crack initiation is at the film-substrate towards the surface to z/t--0.2.
interface ( z / t = 1) under the edge of contact ( r / a = 1 ). At Considering this stress situation a crack may be initiated
this location again a mixed mode stress situation exists that by the high radial tensile stresses which occur in the narrow
consists of high radial tensile and high shear stresses. region around the contact edge. Nevertheless such a crack
will quickly run into a field of high compressive stresses. The
4.3. R/t=2 [R/a=4.Z a/t-0.43] driving force for further crack propagation can only be found
in the high shear stresses which occur at small depths under
Fig. 7 ( a ) - 7 ( d ) shows results for the next thicker film the surface of the film. Again, another possible location for
modeled. The load-displacement curve in Fig. 7(a) indicates crack initiation may be assumed at the interface under the
that plastic deformation in the substrate still influences the edge of contact ( z / t = l and 1.O<_r/a< 1,5) where high
indentation process. Nevertheless, this influence is much radial tensile stresses occur together with high shear stresses.
smaller compared with the previous cases described above Furthermore, a crack may also be initiated by the radial tensile
and compared with the influence due to the elastic deforma- stresses at the second peak especially for the cases where the
tion of the substrate. maximum tensile stresses can be found at this peak (for this
The radial tensile stress on the surface shown in Fig. 7(b) see Section 4.5).
exhibits a sharp narrow peak at the edge of contact. A second
wider but smaller peak occurred outside the contact area at 4,4. R/t=O.67 [R/a.=4.0, a/t=O.17]
r/a ==4. Fig. 7 (c) again shows the curves of the radial stresses
through the film. Around the first narrow peak at 1.0 < r~ Fig. 8(a)-8(d) shows the results on the thickest film stud-
a < ! .5 the tensile stresses decrease rapidly from high values ied. The load-displacement curve in Fig. 8(a) exhibits a
at the surface and become compressive already at small completely elastic deformation behavior with the unloading
depths of zlt < 0.05. Towards the interface the radial stresses curve lying exactly on the loading curve. The plot of the
again become tensile with the maximum value observed at radial surface stress in Fig. 8(b) shows that high radial tensile
the interface directly under the edge of contact. Towards the stresses occur only near the edge of contact. Looking at the
second wider peak the values of stress change gradually to curves of the radial stresses through the film (Fig. 8(c)) it
the situation where the radial tensile stresses decrease from can be seen that the tensile stresses rapidly decrease to
their highest values on the surface until they become com- become compressive at very small depths under the surface
pressive eta depth of z/t = 0.4. of the film. Only small radial tensile stresses occur near the
The shear stresses through this film shown in Fig, 7(d) film-substrate interface. High shear stresses can again be
exhibit about the same shape as in the thinner film (R/t = 6.7) found in a shallow area under the contact edge which decrease
that was previously described. The maximum value still can rapidly toward the interface (Fig, 8(d)), A comparison

0 • • a . . . .

,20

(a) ' 1 0 (b) 2 4 6

11
err [GPa] ,a = 1,ol 10 ~rz [GPa] - - r J a = 1,01
- - - da = t,17 ~j. - - - da = 1,17
. . . . r/a = 1,44 ~ - ~ f ~ . . . . rla = 1,44
/ _-- .... .-2.... . . . . rla = 1,9s
[ .,'- " ~ ...... rla = 2,70
........ ..".'. ...... .;.:... .', . . . . .: .............

i '~ "" .... ~ .... rla = l,se

\ "....~ ...... .~==,70 ..
--rta=3,Ts zlt
-11 i

O(c) 1 O(d) 1
Fig, 7. Resultsof the finiteelementsimulationforR h - 2. (a) The simulated load-displacementcurve, (b) Curveof the radial stress along the surface. (c)
Curvesof the radialstressalongverticallines throughthe filmat differentlocationsrla. (d) Curvesof the shearstress throughthe film.
 E. Weppelmann. M. V. Swain/Thin Solid Films 286 (1996) 111-121 117

°" O'rr[GPa]
10
Pma ~ l mm

-lO j
-20

hmx -30 r/a

00(a) 1 O(b) 3

13 I O" rGPa~ -, r / a = 1 , o
'~rz [GPa] rla = 1,o
! rr t J --- rla= 1,24
10 - -- rla = 1,08
| .... rla = 1 . 2 4
[ .... rla []1,51 ....
....
rla = 1,24
r / a = 1,51
~. ...... r/a =2,17
...... r/a = 2,17

I /'" ~'.
t / ..........
/ ........
z/t
-13 I
0 (e) 1 o (d) 1
Fig. 8. Results of the finite element simulation for R/t = 0.67. (a) The simulated load--displacement curve. (b) Curve of the radial stress along the surface. (c)
Curves of the radial stress along vertical lines through the film at different locations rla. (d) Curves of the shear stress through the film.

between these stresses with those obtained from an infinite 10

thick coating (R/t= O) revealed that the influence of the Grr[GPa] 1
substrate had almost vanished. The stress situation described
above suggests that the only likely location for fracture can
be found close to the contact edge where a crack could be
initiated by the high radial tensile stresses.

4.5, Radialsurface stressesfor different R/h

Fig. 9(a) shows the radial surface stress of three different -100(a) 1 2 3
stages during the indentatton process on the film that was
modeled using a value of 6.7 lbr the ratio of R/t. A fourth 10
and final stage was already shown in Fig. 6(b), It can be seen Grr[GPa]
that the indentation process seems to start with a first peak of
the radial tensile stress directly at the edge of contact. During
further loading of the indenter a second peak of the radial
tensile stress emerges that gradually exceeds the first peak. 0
Upon further loading the first peak vanishes and only the
second peak remains that starts to increase. In order to prove
that the plastic delbrmation in the substrate is responsible for
this behavior these calculations were repeated allowing only
/// r,,
elastic deformations in the substrate to occur. It can be seen Fig, 9. Results of the finite element simulation for RIt = 6,7 showing curves
in Fig. 9(b) that the radial tensile stresses at the surface of the radial stress along the surface for three different stages during the
decrease continuously from the peak at the contact edge with- indentation test. (a) Elastic-plastic deformation is allowed to occur in the
out the occurrence of a second peak. suhstrate. (b) Only elastic deformation is allowed in the substrate,

the material. Furthermore, the stable or unstable extension of

5. Fracture analysis such a crack is possible from whether dKl/dC > 0 where c
means the crack length. For the calculation of the stress inten-
For brittle materials the prediction of the likelihood of sity factor the weight function method can be used. A weight
cracking is related to the stress intensity factor KI for a pre- function exists for any crack problem which is specified by
existing critical flaw exceeding the fracture toughness Kic of the geometry of the component and a crack type. If this
118 E, Weppehuann, M. V. Swain I Thin &)lid Films 286 (1996) 111-121

function is known the stress intensity factor can be simply This weight function can also be used to calculate the stress
obtained from intensity factor Kn for a Mode-II loading condition as long
as a = c/W stays close to zero so that boundary effects can
C
be neglected [ 18 ]. Since the thickness of a thin film is mostly
K,=f dz (l) very small compared to the thickness of the substrate and W
o is related to the entire sample thickness the ratio of a = c~ W
becomes close to zero and the weight function ht(z,c) can be
where ht(z,c) means the weight function and tr(z) the dis-
used to calculate g l l . The weight function ht(z,c) of Eq. (2)
tribution of the stress normal to the crack path, calculated for
is shown in Fig. 11 for a =0. The curve shows that the
the uncracked component along the position of the crack.
stresses near the crack tip will contribute more to the stress
With this method plane problems like through-thickness
intensity factor calculated using Eq. ( 1 ) than the stresses in
cracks can be treated which are characterized by a single
a greater distance to the tip.
parameter, the crack length c. If an external crack is consid-
Of course, the geometry of a circumferential crack as
ered the integration has to be performed along the crack length
developed in thin films by spherical indentation is different
from z = 0 at the surface until z = c.
to the geometry of a one-dimensional crack. Nevertheless,
The advantage of this method is that the weight function
fracture is caused in both cases by a biaxial stress field with
h=(z,c) depends on the geometry of the component only.
stresses acting in a plane normal to the surface and to the
Therefore, if this function is known for a certain component
crack plane. Then, a weight function that was developed for
the stress intensity factor can be calculated for ~ny external
a one-dimensional crack system ntay also be applicable to
loading situation. Since the problem of determining the
the problem of a circumferential crack.
stresses in an uncracked component along a crack can be
Another difference to the case of a plate of one material
solved using finite element analysis techniques the weight
lies in the film-substrata material compound. Since the inter-
function method is a useful tool for the fracture analysis.
face between the film and the substrate further complicates
In this study a weight function for a one-dimensional crack
the fracture analysis the weight function of Eq. (2) can only
in a plate of length L and thickness W (with L > W) is used
be applied within the near surface region of the film, i.e. for
in order to analyse the fracture of the coatings described above
greater distances removed from the interface. Recently, Fett
(see Fig. 10). This function, developed by Fett and Munz
et al. [ 191 developed a weight function for the problem of
[ 18] for a Mode-I loading condition, can be expressed in the
an external edge crack approaching an interface between two
form
materials with different elastic moduli. In their study the crack
faces were loaded with a constant stress distribution. Consid-
h,(z,c) ~ ~ [ I + ~...,~(
~ _ iA,,,,a"
= ~'~:z( I =z/c)"' '] (2) ering an external edge crack in a stifffilm on a softer substrata
(Ef/E, > 1) they found that the stress intensity factor was
where a ~ c~ W with 0 ~ t~ < 0.85. The coet'ticients A..... as always larger as the stress intensity I~lctor calculated for an
determined by these workers are given in Table I. external edge crack in a plate of one material only (Ell
E, = i ). For an elastic mismatch between tile film and the

substrate
¢
% substrata material of Ef/E, = 3 and a crack length smaller
than 30% of the film thickness (c/t ~ 0.3 ) the stress intensity
factor was at the most 7% higher as if it was calculated using
e,,/ E~ = l .
In this study we use the weight function for an external

wf : edge crack in a plate (Eq. (2)) to calculate the stress intensity

factors K, and Kn within the first 30% of the film thickness
using

Fig. 10. Princi tie of the crack geometry used for the fracture mechanics 10
analysis, The fracture behavior of a brittle filmdeposited on a softersubstrate
was analysed using a weight function for an external edge crack in a plate. 8 hl(Z'C)*'~'

Table 1 6

J
Coefficients of the weight function of Eq. (2) as determined by Fett and
Munz 1181 4

m=0 m=l m=2 m=3 m=4 2

n= 0 0.4980 2.4463 0.0700 1.3187 - 3.067 z/c
n= I 0,5416 -5.0806 24,3447 - 32,7208 18.1214 O0 1
at2 -0.19277 2.55863 - 12.6415 19.7630 - 10.986 Fig. 1I. Weight function for a one-dimensional crack in a plate of length L
and thickness W ( w i t h L > W) for a=O.
 E. Weppebnam,, M. V. Swain I Thin Solid Films 286 (1996) 111-121 I 19

C
K~ +/3/(i~n= K~.vp, = / ~ c for Kz>__0 (6)
x, = f .Cz)h, Cz,c) dz (3)
0
and
¢
/3K~,=K~pp, =K~c for K, < 0 (7)
Kn = f ~'=off(z)ht(z,c) dz (4)
0
In this, Kt apptmeans the equivalent value for the stress inten-
sity factor whereas K~c means the fracture toughness for a
with Mode-I loading condition. The factor/3 considers that usually
Ktc~Knc resulting i n / 3 > 1 for K i c > K a c and i n / 3 < 1 for
/ ~'=(z) for K~>0 Ktc<Knc (see Fig. 12(b) for/3> 1).
~',,.off(z) = I,r~,(z) +#try(z) forKt<0 (5) The following results were calculated using the above
stress curves of Figs. 5-8 and using values of 0.5 and 1.44
where O'r~(Z) and z,~(z) are functions for the radial stress and
for the friction coefficient g and the factor/3 respectively.
shear stress respectively ( see Fig. 12 (a) ). Eq. (5) considers
Fig. 13(a) shows the curves ofK~ appl versus c/t for the two
that the shear stress that accumulates at the crack tip will
cases of RIt = 20 and R/t = 6.7 using the stresses o',~(z) and
decrease due to friction as soon as the crack sides are pressed
~'r,.(Z) at the locations of r/a = 1.24 and r/a=2.04 respec-
together by comlzressive stresses which will occur at the
tively (see Figs. 5 and 6). It was found that the influence of
moment where K~< 0. In this equation,/s, corresponds to the
Kn is almost negligible due to the small amount of shear
coefficient of friction between the crack sides.
stress. It can be seen on these curves that the values of Ktappt
For the fracture analysis of the films the stresses that are
are already high in the near surface region indicating that
most likely to be responsible for the initiation of a crack will
even very small pre-existing flaws in the surface of the film
be considered. The functions for tr,(z) and ¢,,,(z) were
may be sufficient to initiate a crack that can lead to the
obtained by fitting a polynomial function to the stress curves
observed fracture through the film.
considered in this analysis. A maximum degree of 10 was
The situation is different for thicker films, i.e. for smaller
used for the fitting procedure so that the coefficient of deter-
values of R/t. Fig. 13(b) shows curves of Kt avp=versus c/t
mination R2 between the polynomial function and the stress
for R/t= 2 and R/t=0.67 using in both cases the stresses at
curves was in every case better than 0.99. For the analysis it
the contact edge where r/a = 1. Both curves exhibit a discon-
was further assumed that the substrate is thick compared to
tinuity near the surface. This marks the point where K~
the thickness of the film so that ot becomes zero. Curves of
becomes smaller than zero and Kt= decreases due to friction
Kn and Kn versus crack length c were obtained by a repeated
between the crack sides leading to the observed discontinuity.
numerical integration of the right hand side of Eqs. (3) and
(4) for different values o f c starting from z = 0 on the surface
to z = c at the crack tip (see Fig. 12 (b)). The integration was Klapp I [MPa4~]
carried out until a value of clt = 0.3 was reached.
In order to superimpose the curves o1' Kn and Kit into one
curve of K~,pp~versus crack length c, the I'racture criterion of 20
the energy release rate is used which leads to

10
Ca) q ..... ¢rrr(Z)
.~,~7~'q'zlz)
eli
X~rzCZ) 00Ca) 0.1 0.2 0.3
~KI<O "~
lsl Klappl [MPa~r~]
z/t'
(b) 0
KI

c !t
KII
zlt °o Sb) o11 -o12 ?.3
Fig, 12. Principle of the fracture mechanics analysis. (a) The distribution Fig. 13. Curves of the stress intensity factor Kt at,v1calculated within the first
of the stresses along a crack of length c. (b) Curves of the stress intensity 30% of the film thickness using (a) R / t = 20 and 6.7 as well as (b) RIt =2
factors along a crack of length c. and 0.67.
120 E. Weppelmann. M. V. SwaJn / Thin Solid Fihns 286 (1996) 111-121

Fig. 14(a) and 14(b) shows the influence of the coeffi- a pre-existing critical flaw reaches the fracture toughness Kc
cient of friction/~ and the factor/3 on the curve of KI appt of the coating material.
versus cltrespectively for the case ofR/t = 2. The coefficient This results correlate well with the fracture behavior
of friction was varied from 0 </z < 0.95 whereas fl was varied observed during spherical indentation tests on TiN and TiAIN
from 0.64 </3 < 1.69 according to the recommendations of films deposited on various substrate materials. The fracture
Munz and Fett [20]. Both parameters exhibit a great influ- behavior described above was observed for ratios of R/t
ence on the curve of K~~pp=. between 0.6 and 13 using indenters of different radii between
Two different cases for the fracture behavior of thin films 2 and 35 I~m on films which were 2.7 to 4.5 I~m thick. At the
during spherical indentation tests can be recognized in Fig. occurrence of the first crack the ratio of RIh ranged from 5
to 87 for indentations carried out with a 2 and 35 I~m radius
13: ( 1) for thinner films, or greater values of R/t respectively,
indenter respectively. The SEM picture of an indentation in
a crack will be initiated and driven by an almost pure Mode-I
a TiAIN coating shown in Fig. 3 exhibits two circumferential
loading; (2) for thicker films, or smaller values of R/t, the
cracks that lie within the area of contact. The first crack
fracture behavior is dominated by a Mode-II loading apart
occurred at a depth of h = 4 0 0 nm (see Fig. 2) leading to a
from the nearest surface region where a mixed mode loading
ratio of R/h -- 87. This indicates that the first crack happened
occurs consisting of Mode-I and Mode-II.
near the contact edge where high radial tensile stresses occur
Between these two cases an intermediate situation exists
during the initial stages of the indentation process (see Fig.
where it cannot readily be clarified where fracture will occur.
9(a)).
A first evidence for this situation can be found in Fig. 7(b)
where the radial tensile stress on the surface exhibits a second
maximum outside the edge of contact. Fig. 1 l(a) further 6. Conclusions
indicates that this second maximum gradually exceeds the
first maximum at the contact edge during the course of the This study has demonstrated that with spherical diamond
indentation process. Therefore, it seems obvious that a situ- tipped indenters one is able to measure a critical load for the
ation exists during the indentation process where fracture may first circumferential crack through a thin protective film. In
occur either directly at the contact edge or in a greater distance order to analyse the stresses which are responsible for the
from the contact area where the second maximum occurs. observed fracture behavior a finite element analysis was car-
Whether fracture occurs either at the first or at the second ried out that considered not only the elastic deformation of
maximum depends where the stress intensity factor Kt ,,ppt at the spherical tipped indenter but also the elastic-plasticdefor-
mation of the substrate material. In this analysis the film
thickness t was varied in relation to the indenter radius R
20
'KI appl [MPa./~'] using values of 20, 6.7, 2 and 0,67 Ibr the ratio of R/t.
16 It was Ibund fi)r the thinner films (R/t= 20 and 6,7) that
high radial tensile stresses occurred outside the contact area.
10 These radial tensile stresses decreased from their maximum
values at the surface to become compressive but not until a
6 depth of 50-60% of the coating thickness was reached. It was
demonstrated that this stress situation is caused by the plastic
0 deformation in the substrate using simulated Ioad~lisplace-
clt ment curves and a comparison of curves of the radial surface
O(a) 0.1 012 0.3
stress for both, an elastic-plastic and a pure elastic substrate
behavior.
For the thicker films (i.e. R/t= 2 and 0.67) high radial
Klapp I [MPa,/'~'] 13 = 1,69/,, .''~ tensile stresses were tbund in a shallow region on the surface
,o near the edge of contact only. Except of the. thinnest film
studied (R/t=20) high shear stresses were found in the
middle of each film with maximum values directly under the
edge of contact.
A fracture mechanics analysis was carried out within the
first 30% of the coating thickness using the weight function
o/t method in order to calculate curves of the stress intensity
00-(b) 011 "r 0.~ 0.3
factors K~ and Kn versus the ratio of clt where c means the
Fig. 14, Curves of the stressintensity factor Kz=~=,=calculated for the case of
RIt - 2 within the first 30% of the film thickness varying (a) the coefficient crack length. Using the fracture criterion of the energy release
of friction tt between the crack planes from 0 to 0,95 and (b) the factor/3 rate both curves were summarized into a single curve of
of the fracture criterion of the energy release rate from 0,64 to 1,69 according K~~p= versus clt. It was shown that for R/t= 20 and 6.7 the
to the recommendations of Munz and Fett [20]. situation was dominated by a Mode.-! loading situation and
 E. Weppebnann, M. V. Swain / Thin Solid Films 286 (1996) 111-121 121

that fracture may already be initiated from very small pre- [4] J. Menc~ and M.V. Swain~Muter. Forum, 18 (1994) 277-288.
existing flaws in the film surface. For the cases where R I t = 2 [5] T.W. Wu, R.A. Bum, MM. Chen and P.S. Alexopoulos, Muter. Res.
Soc. Syrup. Proc., 130 (1989) 117-122.
and 0.67 fracture could be caused by a pure Mode-II loading [6] M. Samandi, T.J. Bell and M.V. Swain, Muter. Res. Soc. Syrup. Proc.,
condition. Only for very small pre-existing surface flaws frac- 239 ( 1991 ) 355-360.
ture could be initiated by a mixed mode loading situation [7] J.C. Knight, AS~.Whitehead and T.F. Page, J. Muter. Sci., 27 (1992)
consisting of Mode-I and Mode-II. The results were in good 3939-3952.
[8 ] A.J. Whitehead and T.F. Page, Thin Solid Fihns, 220 (1992) 277-283.
agreement with the fracture behavior observed during spher- [9] J.L. Loubet, J.M. Georges and Ph. Kapsa, Mechanics of Coatings,
ical indentation tests on thin brittle films. Elsevier, Amsterdam, 1990, pp. 429-434.
[10] G.M. PharL D.S. Harding and W.C. Oliver, Proc. NATO-ASI.
Portugal, June/July (1992), Kluwer Academic, Nethedand, 1993, pp.
449--461.
Acknowledgements [ I l l V.A.C. Haanapple, D.v.d. Vendd, H.S.C. Metselaar, H.D. van
Corbach, T. Fransen and P.J. Gellings, Thin Solid Fihns, 254 ( 1995 )
The Authors wish to thank G. Rizzi and E. Diegele for 153-163.
their assistance with the finite element analysis and T. Fett, [12] E.R. Weppelmana, X.-Z. Hu and M.V. Swain, J. Adhesion Sci.
Technol., 8 (1994) 611-624.
D, Munz and J. Menc~ for discussions and their comments [ 13] M. Shiwa, E.R. Weppelmann, A. Bendeli, M.V. Swain, D. Munz and
on the manuscript. T. Kishi, Surf. Coatings Technol., 68/69 (1994) 598-602.
[ 14] M.V. Swain and L Menc~, Thin Solid Films, 253 (1994) 204-211.
[ 15] S. van der Zwaag and J.E. Field, Philos. Mag. A, 46 (1982) 133-150.
[ 16] H. Djabella and R.D. Arnell, Thbl Solid Fihns, 213 (1992) 205-219.
References [ 17] H. Djabella and R.D. Amell, Thin Solid Films, 213 ( ! 993) 98- ! 08.
[ 18] T. Fett and D. Munz, Stress hztensity Factors and Weight Functions
[ 1] M.F. Doemer and W.D. Nix, J. Mater. Res., 1 (1986) 601--609. for One-dimensional Cracks, Forschungszentmm Karlsruhe,
[2] W.C. Oliver and G.M. Pharr, Z Mater. Res., 7 (1992) 1564-1583. Dezember 1994, KfK 5290.
[3] J.L. Loubet, M. Bauer, A. Tonck, S. Bec and B. Ganthier-Manuel, [ 19] T. Fett, E. Diegele, D. Munz and G, Rizzi, personal communir'aions.
Prac. of the NATO-ASI. Portugal, June/July (I 992), Kluwer Academic, [ 20 ] D. Munz and T. Fett, Mechanisches Verhalten keramiseher Werkstoffe,
Nethefland, 1993, pp. 429-447. Werkstoff-Forschung and -Technik 8, Springer Verlag, Berlin, 1989.