ELSEVIER Thin Solid Films 312 (It;t)n) 24(i-248

Simulation of Berkovich nanoindentation experiments on thin films

using finite element method
M. Lichinchi :', C. Lenardi "'*. J. Haupt ~', R. Vitali h
"' ('nmmi.~.sim~ o]'the l;'urol~eu. I hdma, I..~titttte.for Adt'~lm'¢d M(llerials, ,Inint R('.~carch C~'ntrc, 1-2102(I I.v.'a ( V¢D. It.l,v
u Hihhitl. K.rl,s~,.t .mtSoren.sen It</flu, V,h, ('{'rloan I, f-20149Mihnm, II.lv
Received6 May 1097: aeccl3tcd4 AtJ~ust 1997

Abstract

The Finite element technique is applied for studying the very complex stre:;s-strain Field of thin hard coatings subjected to a
hast:indentation process. Berkovich indentation experiments were simulated with the ABAQUS Finite element software package. The
investigated system was titanium nitride on high speed sleel as an exampfc or a hard film on a softer st.bstrate. The tmmerical analysis
allowed the plastic deformation history dtning intle,ltati(m to be I'nlh~wed. in particular, it was possible to correlate the onset of plastic
deformation in the substrate with the shape of the loading curve, The system was ~imulaled by ;.m axisyn)tnetric nlotlel in which tile
conical indenter has the same contau't area its the Berkovich indenter, A six-fold symmetric three-dimensional model was also defined for
testing the suitability of the previous model. Tile indenler was modeled either as a rigid surface or as a delkwmable tliamotld tip.
Comparison between the experimental data and nttmerical resulls demonstrated that tile I'inile elemet)l approach in capable of reproducing
the loading--unloading behavior of a nanoindentation test. The film hardness of TiN/HSS specimens was numerically calculated for
different indentation depths. It was shown thai the presence of the substrate affected Ih¢ hal'thtess IlteaStlt'eltletit l~)t" relative indentation
depths greater than about t5q- of tile filrn ihickliess. ,O 199g Elsevier Science S.A.

Kcvu'ord~: J:iltile el¢llleU1[ nlelhtld, Berkovich namfiu~denlaitmllproccs,,: TiN/HSS

I. Introduction material having an internal hydrostatic pressure. Johnson

[3] added to this approach ihe effect of the tip geometry.
The mechanical surface prop,.riles of tnany materials
However. all the nroposed models cannot describe the very
can be improved by "Jepositing .hppropt'iate coatings, in
cornplex stress and strain fie!d produced during the inden-
particular with respect [o wear resistance, friction coeffi-
tation process. Since the induced plastic defortrmtiotl de-
cient, hardness, etc. Local dek)rmations of coated surfaces
pends on the path through which each indentation step in
produced by tribological interactions can result in substan-
reached, it sllould he very usct'ul to be able to analyze the
tial d:mmge. Thus. it is important to quantify the resistance
deformation history.
of the material to such damage. For this reason the evalua-
Some inwestigators have studied the indentation pl'oces.,,
lion of the hardness its obtained frotn indentation measure-
using the numerical approach of finite elemenll nlethod.
ments is of fundamental importance. Elastic modulus and
Cai and Bangert [4] studied with this nlethod the extension
hardness are the two properties that are more frequently
of the plastic deformed zone in relatiol] to the ratio of the
measured by the load and depth sensing indentation tech-
penetration depth to the filnl thickness d / l , and deter-
nique. Theoretical analysis of gener:d indentation problems
mined the erl'cct of the substrate on the measured hardness.
has received great attention I'rom many investigators, A
In tile case of soft filrns on hard stlhstl'ates they found thai
few models are based on the classic slip line thcory for
this effect wits still negligible up to d / t × I()0 "- 3()'~. 011
rigid-plastic solids [I]. A new approach was introduced by
the contrary. Ii)r hard l'ihns on softer suhstrates, the plastic
Tabor [2] who analyzed the plastically delk)rmcd zone as
deformation extended easily into the sttbslrate, and the
the expansion of a spherical cavity in an elastic-plastic
measured hardness wits tnodil'ied even for d / l X I()()--
109;. Sun el al. [5] employed an axi,~ymmetric FEM model
('orresDmdin~ ;tuthor. to simulate a hard coalin~ Oll ~.t sol'lcr stlhstl';.lle, A conical

(x)4()-6ou(I/98/$10.(~) r t908 i.:lse~,ier~¢iellce .~.A. All rights rencl".etl.

i'11 s()040-6()t)()( 97 )0l)77,9-(')
 M. Lichinchi et al. / Thin Solhl I"ihns 312 ( 19t),~; 240-248
indente," having the same projected area-depth function as
the Berkovich indenter was assumed. The nanoindcntation
process for various coating-to-subs,rate yield strength ratio
was analyzed. Moreover. the effect of the indenter tip
radius was taken into accotmt. Sun ct ai. [5] deterrnined
that an increase of the yield strength ratio or of the tip
radius reduced the critical ratio (d/t)c, il for which the
hardness measurements were not affected significantly by
the substrate. A three-dimensional FEM analysis was per-
formed by Wang and Bangert [6] who investigated the
behavior ol" coated systems during a Vickers indentation
process. The rest, Its showed that the first part of the
loading curves closely followed the behavior of the bulk
coating and from d/t x 100 = I0'% the effect of the sub-
strafe became evident. A first example of comparison
between FEM analysis :rod exl')erimental results was pre-
sented by Bhattacharya and Nix [7] in which they simu-
lated a sub-micrometer indentation test. They verified that
the finite element method could be an effective tool for
simulating hardness measurements.
in our work. we used the finite element method to
simulate the nanoindentalion process. At first we compared
the experimental load-depth response of titanium nitride
thin films on high speed steel subs,rates with numerical
results. Successively. we studied the el'feel of the subs,rate
on the. hardness measurenlents. Due to ,he complexity of
the phenomena involved in tile indentation process, we
used the FE program ABAQUS [8] which allows effective
modeling of non-linear problems such as the materials
properties, the contact between two bodies .'rod the large
delbrmations of the material under tile indenter.
|:ig, 1, .%thematic repr¢,s¢i;talJolt of Ioad-dJ,sl)la~.¢illeM data for a ||ai~oJltd~.'llt0.lio|~ 'J~.rwcl'iil'l.L'lll, l~qt,,~,: l'l'ta\J|11t|fl'l apptl~d load; h,..,~: tl~c |i~axJm~ii~)
di.'.lllau'en|ei|l: h t: iii|a] |'..'|K'tralioi~ depllv d IJ/dh~,,~l,,,,d: ,,.h~pe ~fl IIK' kmh~adhlg cm".e,
241
2. N a n o i n d e n t a t i o n m e a s u r e m e n t s
The nanoindentation technique allows Young's modulus
and the hardne.ss of thin films to be evaluated. In this
section, we describe how a nanoindentation me;tsurernent
is pefforrned and how the experimental results are elabo-
rated for determining the mechanical prol:erties. Nanoin-
dentation measurements are pccformed und,;r a constant
load rate control. When the final depth is reached, a
const:mt load is maintained to allow for pos.,Jble creep
before t!~c unloading with a constant displacemm,* rate is
perform, d. in Fig. I, a schematic draw of al~. inde~.;ation
Ioad-disFlacement curve without the constant load seg-
rnent is ;hown,
As reported by Oliver and Pharr [9] and Brotzen [10]
the effects of a non-rigid indenter on the load displacement
behavioT can be taken into account by defining an effective
modulus E~
t I - v2 I - v,-'
E,, E E,
where E is the elastic modulus and v is the Poisson's ratio
of the specimen, and E, and v, are the same parameters
for the iadenter, b.; is evaluated l'rom the nunoindentation
measurements according to the following equation
v"~r (d P / d h),,.,,,,,a
'% = 2- " (2)
where ,..J is the indenter load. h the penetration depth and
(dP/da)u,,,,, d is the slope of the unloading curve evalu-
ated at tile position ot" maximum load. A i. the contact
242 M. Li,'him'hi el al. /
area and ~ is a dimensionless parameter related to the
geometry of the indenter. In the case of a conical indenter
/3---I.
For evahmting the elastic modulus E,. the slope
(dP/dh).,,h,,,, j and the contact area A should be deter-
mined precisely. A least mean square fit to q(Y;~ of the
unloading curve is made according to the hypothesis that
the unloading data will be better expressed by a power law
(It--~,,)'"
P = P'""" h,,,-~,~-S/,,.
P.,,,x. h,,:,~ are the maximum load and the maxinlum
displacement respectively, while the final penetration depth
h r and the exponent m are the parameters to be fitted. Eq.
(3) is than analytically differentiated for determining the
slope (d P / d h)..=,,, d.
The contact area A is given as a function of the contact
depth h~. The contact depth at maximum load is then
h~. =/,,.,, - ,~( h,,,,,, - / , , )
where e = 0.72 Ibr a conical indenter as given by Sneddon
[11]. The expression for the contact area lbr a Berkovich
indenter is usually approximated by the lbrmula
7 muhi-point constraints (MPCs type linear) are introduced
A( h. ) = 24.5h~.' + ~ C, h~.l/"'. (5)
where the tlr~;t term gives the contact area of an ideal
indenter whereas the terms pro.sere in the ~;um t,tkc inI,~
account geometrical deviam;ns due to the tip rounding.
The Young's modulus E is obtained from Eqs. (I) and
(2). and the hardness H is given by the well-known
relation
H= ~ .
A disl~lacerncnts along .v and v direction, are COlretrained.
l Z
Fig. 2. IV1¢sh of lhc ~qlol¢ sample wilh the imlcnlcr m~dclcd a.~ u inovablc rigid .,,re'face,
7hi. Solid l'7h,s 312 ¢1998J 240--24,~'
3. FEM modeling
hi the present work. we have studied the nanoindenta-
tion process e r a TiN coating grown on a HSS substrate.
The nanoindentation measurements have been perlbrmed
with the deptll sensing Nanoindenter ii of Nano Instru-
ments equipped with it Berkovich diamond tip. We have
simulated the process using an axisymmetric model which
allows mesh definition with a restricted number of degrees
of freedom. However. we have verified il" this modeling is
(3) appropriate by performing an analysis with a three-dimen-
sional nlodel.
3. !. A.visymmetric mmh'l
In order to define an axisynlmetric model, we have used
an equivalent conical indenter with a semi-apical angle of
0 = 70°30 '. This system has geometric and loading sym-
metry around the axis of the indenter. The specimen is
rnodeled with 2635 4-node axisymrnetric reduced integra-
(4) tion elements (CAX4R element type [,~l]). as shown in Fig.
2. The indentation region is very small with respect to the
size of the sample. A high mesh refinernent is used for
modeling the large delormation area. In the outer zones
lot interfacing one element with two adjacent elements to
rcduce the total number of degree~; of freedom. Finally
semi-infinite elements (CINAX4 clement type [8]) resem-
ble the far field dornain in the radial direction. The ele-
ments at the interlayer between the film and the substrate
are reduced in height to be able to detect more accurately
thc behavior of that zone. The imposed geornetrical bound-
ary conditions arc: the nodes along ti~e axis of rotation can
move only along such an axis. i.e.. the v axis. and all the
(6) nodes on the bottom of the mesh are fixed, i.e.. the
 M. l.ichin('hi et al,/Thin Solid Films 312 f1~98) 241)-248 243

quent steps: loading and unloading. During loading, the

rigid surface or the modeled tip moves along the v direc-
tion (see Figs. 2 and 3) and penetrates the specimen up to
the maximum depth; during unloading, the tip returns to
the initial position. At each depth increment, the program
makes many iterations according to a specified conver-
gence rate to reach an equilibrate and congruent configura-
tion.
Purely elastic deformation takes place onl~ during the
beginning of the indentation process. The Mi,~,s yield
criterion is applied for determining the occurrence; cf the
plastic deformation. The equivalent Mises stress is given
by the expression

~rl - ~r~_)" + (~r~ - ~r~)" + (~r~ - ,r, )"

( ~ m i ",c'-, = 2 "

Fig, 3. Detail o1 the indentation region with the indenter modeled as :m
elastic-plastic tip.
An important feature of ABAQUS is its capability to
model the contact between two bodies as a sliding through
contacting surfaces, which arc in our case the indenter
surface and the specimen surface. From the initial geome-
try the nodal gaps between the surlaces are defined. Dur-
ing the analysis, the program controls the variation of the
nodal gaps. in particular whenever the distance between
the indenter and the specimen becomes zero--gap closure
~ t h e contact takes place and an external reaction lbrce is
exerted on the nodes involved in the contact. The contact
constraint is enlbrced by tile definition o1" the "master' and
the 'slave' surfaces' only the master surface can penetrate
into the slave surl':~('e and the contact direction is always
taken as being normal to the rm~ster surface. We have
chosen the indenter surface as the master surface due to
the larger stiffness of the indenter with respect to the
specirnen. In Fig. 2 the indenter is represented by a rigid
movable surtace. Since the coating is very hard, wc have
also modeled the tip with axisymmetric elements for tak-
ing into account the stiffness ot' the indenter. This mesh is
shown in Fig. 3.
The friction coeMcient between the tip and the speci-
men surface is assumed to be zero, because ill tlbe case of a
hard coating on a softer substratc, like T i N / H S S system,
the friction has a negligible effect on the nanoindentation
process. i
Coaling a n d substrate are as:,umed to be initially stress
free and in perfect contact duriug the indentation process.
Both the TiN roaring and the HSS subslrate arc as-
sumed to be homogeneous and isotropic and having a
perfect elastic-plastic behavior.
The indentation procedure i.,' simulated by two subse-
I K, Malnuda. I)l'i:'atc ¢oillintltfit.atilltl,
(7)
where tr,, tr~ and tr3 are the three principal stresses.
Whenever (rm,,,.` reaches the yield strength tro, the mate-
rial begins to deform plastically.
3.2. Th ree-dimensional mode/
The Berkovich indenter is a triangular-base pyramid
having a six-fold symmetry. The load is applied along the
axis of the indenter, thus the load s),mmetry is the same as
the geometric one. For these considerations, a thi ee-dimen-
sional model is defined only by one sixth of the entire
system. The specimen is modeled with 6925 B-node re-
duced integration elements (C3D8R element type [8]) and
with senti-infinite elements (CIN3D8 element type [8]).
The three-dimensional mesh is reported in Fig. 4. The
large deformation area is modeled with elements smaller
than these in the outer zone. We used a coarser mesh with
respect to the axisymmetric model in order to limit the
degrees of freedom. Due to the fact that in the axisymmet-
ric analysis the results lbr a rigid and for a detbrmable
indenter are very similar, as described below, we have
modeled the indenter with a rigid movable surface.
loading
h~
Displacement
Fi~. 4. Three-dh~lcnnional mode1. The Bcrkovidl indenter ha.', a six-I~ld
' :||R.t II1¢ load i,, applied ~don,e Ih~." axis L~I the illdl211l¢l', '1"11¢mesh
~,)'lllln|r~ll~)
is dk'lined old x l~r oll.t2-Mxlh of the .,,xstem.
244 -], .I, b
M. Lit'him'hi ~'i ot. / lTm~ .'hdid I.ilm.~ 312 119~),'ft _40-o_4,~

Table I
Material pr't~perlie.~ of TiN, HSS and diaillond u.~cd in t~te liHil~: eleme~,l ',imttlalitm
Yt ,,;,;~'.~ Young'.4 ,m+dtJlus I:' Ikfi~.,,tm's Yield .strength tlardncs.~
modtdtlS ((;P~) rigid indenter ratio ~, Y (GPa) t l ((-]P:0
E ((;Pa)
def~;rmable
intler~fcr
'FiN 5,'u-nple # I 427 305 0.25 13.5 27
TiN Sample # 2 45(I 3111 0.25 14.5 27
ItSS 21 X, 218 0,30 1.8 5
Diamond 1141 ().(17 35.7 08

I ' .... I ; | ~ I ' I " I " I "T'-- - -

40 --,~ --. e x p e r i m e n t a l data

.....~ - - n u m e r i c a l data: d e f o r m a b l e i n d e n t e r
- J - × - - n u m e r i c a l data: rigid i n d e n t e r
30

E 20 Sample#1
"o
o
_.1 10

i , _ _ 1 , I , I i I , I .~. , I •

o.oo 0.05 o.m o.15 o.2o o,2~ 0.30 0.35

Displacement (~tm)
Fig. 5. l,oading-unl~adh]# cur~c i'~r Sample # I: c~',upari~{m bcl~een eXl~ei'inlelllald,tt;.t(.~1, i~lld ~imuh~lion re~LiIls, dclt,rnlah' ' diamond imlenler ([])
,u~d r i g i d i n d e n t e r ( x ).

I ' I T T ' ..... I "' ; I

20
.....~ - - e x p e r i m e n t a l data
- - ~:. - n u m e r i c a l data: d e f o r m a b l e i n d e n t e r
.....x - - nt,merical data: rigid i n d e n t e r ~z~;ff"
. ~
-7
15

Z
E: lO Sample#2 ,,~Y/" ff

--L----.~- ..... I ..... , .I i I , I

0.00 0.05 0,10 0.15 0,20
Displacement (!um)

Jq~. 6. I , o a d m . ~ - - u r l l ~ ; i d i n ~ cuP, c f o r S a m [ t i c # 2 : ~ ' o t n l l a t i 4 o l l b e t w e e n ~per'ttY~etfLal dab.i ( ~ ) . ;.mtL ~,it111it;.LLiu,rl r¢~rLIFi>,, d,el,L~.ttnable ,di[tf~'Lm,lld it~ldetlfet' ( L 3 )
;llld rigid indenb'r ( s ),
 M. l,ic'hi/whi et al. / 77aht Solid l.'ilm.~ 312 ¢ 1998J 240- 24t~ 2~5

4. Resultsand discussion ell results arc shown for Sample #1 and St,-~ple # 2
respectively.
4. !. Crmtpurison with e.tperimentai data The agreement between ~lte expe,imental results and the
finite element calculations is satisfactory, in particular in
Tile nanoi=ldentation experiments have been performed the first part of the unloading curve where the Young's
on two magnetron sputtered films grown with diffc,'ent modulus ix evaluated.
deposition parameters. Two coatings with a thickness of The loading curves show a larger deviation than the
2.6 /zrn (Sa,nple # 1 ) and 3 , 0 / z m (Sample # 2 ) have been unloading curves. This may be due to differences in the
studied by nanoindentation using penetration depths of 0.3 actual and assttrned yield strength or due to the use of a
/xm and 0.2 ~rn respectively, i.e.. 12% and 6% ot" the film constitutive model of materials like the perfect elastic-plas-
thick,ross. tic one without work hardening rate. Other causes of the
Tile Yotmg's modulus E of tile coating introduced in disagreement could be the rounding of the tip as a result of
the analysis is determined from Eq. (1). it depends on the wear [i 31.
stiffness of the tip since E r is evaluated from the nanoin- The comparison between the results Ibr the two differ-
dentation experiment. In the numerical analysis, we use ent models of the tip shows no relevant differences. The
either a rigid surface or a deformable tip as an indenter only significant discrepancy is the value of the rnaximum
model. For a rigid indenter. E,--', ~c and the last ternl of load. which is slightly higher in the case of tile deformable
Eq. (I) can be neglected, whereas tbr a delk~rm;tblc inden- lip. This is due to the partial absorption of the delbrmation
ter E, has been taken to be equal to the elastic modulus of energy from the indenter.
diamond. The input values of E for tile FEM analyses are The three-dimensional model with perfectly sharp
reported in Table I. Bcrkovich indenter has been used for testing the validity of
Tile values ot' yield strength P l'ourld in literature for the axisymmetric model. In particular, we want to verily if
TiN [4.6] wcrc too low for the perfect elastic-plastic ruotlcl the use of a pyramidal indenter could better reproduce the
that we have considered, in fact, Ioading-ullhniding curves experimental loading curve. As suggested by tile axisym-
obtained using those vahies do not faithfully reproduce the metric analysis, no relevant differences are apparent be-
behavior ot" the exl~erimental data. In pariicuhir, the inaxi- tween the two models of the i,~denter. Therefore. we have
mum load is lower. We have tried to improve the agree- chosen to model the tip as a rigid surface in order to
ment by increasing the yield strength of the film. The best restrain the degrees of freedom.
value has been Ik)tiild tO be -~ 14 GPa for both samph.,s as The hmding-unloading curve of Sample #1 has been
shown in Table I. This result is consistent with the linear simulated with the three-dimensional model, in Fig. 7 the
dependence of H / Y verstts E/}' as reported by Tabor results of the analysis are compared with the correspond-
[12], For materials having a ratio E / Y of the order of IO. ing responding data of the axisymmetric model. The curves
H / Y "- 1,5 and for I"/Y greater than I(10, H is about 3 Y. are practically ktentical indicating that the axisymmetric
in our case E / Y = 32 ;.|lid the ratio t t / Y -'- 2 gives a value model with a conical indenter, which has the same area
lying on the straight line within the indicated limits. function of the real tip. is an effective tool lbr simulating
in Figs. 5 and 6. the experimental data and tile nunleri- nanoindentation procedure with a Berkovich indenter.

( ' I ; 1 ' 1 ' I ' I ' i '

40
×= axisymmetricmodel ~/~.j
-.-= .... three-dimensional model
30
z
E 20

0
..J
t0

mim>e~'-" ~'-..~< ...................... x ............. × ...... ×. - .>n,--~,

, i , | ~ I ~ L , I , =i

0.00 0.05 0,10 0.15 0.20 0,25 0,30 0,35

Displacement (~tm)
I'i~. 7. |.~,~adilt~--titth~idit|~ ¢.'til'~~' l~,bt~ ~tti'lpl¢ # i: ~.'OIUl'K|t'i~,OIIbL'tWL'en ~L\I',~ ||lll"l~.'t|'iL." model ! "- ) and tt~re,~'-diltl¢|p, ioilai t'llodel ( ~ ) ,
240 M. Lirhi~whi ~,/ ~1. / Thin S¢~liel I~'ilm.~' 312 ¢1~¢,~/¢~240-24A'

' I ' I ~ I ' I ' I ' ] ' :i ' I 'I

210
--^-- bulk TiN specimen /~
180 --.-- T i N c o a t i n g (2 I.~m) o n H S S s u b s t r a t e
• ,¢", d ,'
1,50 ]
• (d;t)x100=17Vo
~" 120 ~ ..i

E <,,,>.,oo:~,%/ >~.o'" /.'

(d/t)x100=13Yo / / ^2'; i. ,~ ? "
-
O
oo /./
30 ~

i t , ]1 , ~ ~ J / ,LI 1 • I , ~ , 1 ,

oo 0.~ 0.2 0.,~ 0.~ 05 0.6 0.7 0.8

Di.e;placement (i.~m)
Fi~. 14. l.ll;idin~-unht,idin; ciirvc: ~Oillpmi.~,il bt'lwecn hLill~ T i N ~,pcc-inlc'n {.~) lind TiN rilln (2 # n l ihiekll¢.~) llll lt,~S ~tihMrillc' I t ).

I = I ' I ' I '

210 ~ ' i , I , 1 ' i ,
. .~ =
TIN //~?
180
F /' )~ .
150
a) //i,g j, .
Z 120 ./ d i
E
90

O
._1 6O ..,,'; / / /
30 o -o~.~
" . . . . ...... " </ /- - ) { 1
?

,~.X.:rCm:~;,L~__.k2:, '~ _.>~ ,' o -jTZ" ........... ;.. ........ *SL- -.,;--c, / .~

, I ~ I , I , t , L r t , I i , i

0.0 0.1 0.2 0.3 0.4 0+5 0.6 0.7 0.8

Displacement (~tm)

210 ~- ' ' ' t , t i i , i i 'J ~ ,

18o I'r TiN / HSS

150 r b) ..~,,,,~

r
90
~o ~i~'S ~'
I
-J' ^" ,^/ i' /

,..~=,=~_~Z,,,~'2 .... ..>2_ , " ...... ,,("...... /

I , | , I ~ I , I , i , I , I

0,0 0.1 0.2 0.3 0.4 0.5 o6 o+T 0,8

Disp;acement (l.Lm)
Fig. ~J. ~', r,~..,,, i,~tlloindentiltitm lm,C~.',,w ,, with dill~.'r~.'.l Iim;I pcnL.,tratioll depth: (il) lot hldk "f'iN: (b) Ior ] i N / I I S S .
 M. Li('him'/d et ,I. / 77#n Solid l"i/m.~"3/2 (/99,++'I 240-24,'+' 247

25 ~ ~ ~ I ..... I . . . . . . . . . . . I . . . . . . .i . . . . . . . . . I

~ '20 -,.....

~n 15 ---" ..... TiN

E .... o - - T i N / H S S
lO

L i I , I ~ I , i * 1 ,

~0 ~ 2o 25 3o 35 4o
penetration depth / thickness (%)
Fig. i(), Ct+nnpari.,,tm bt211+~.l~el'~Ihc t'la.rdn¢,,xul' bulk "FiN i|ll<.lof +FiN/FISS u.,, a fulldiOl'~ of the rati,t~ d/t.

4,2, Load r e m ' n s I~elu,lration d e p t h fin" ('oaled .,,"n~'tems fore, t h e h a r d n e s s evaluation is strongly affected by the
ratio d/t. For a quantitative evaluation of the error on the
Wc have used the axisyrnmetric model described previ- hardness n'neastnrcn~ents due to the substrate stiffness, we
ously for studying the very complex stress-strain field have perforated a series of numerical analyses for both the
induced by the indentation, in particu!ar, we have studied bulk TiN and the T i N / H S S system with different final
the effect of the substratc on the distribution of Ihe plastic penetnltion, in Fig. 9a and b the load versus depth tbr the
d e f o r m a l i o n f o r coated systems as a function o f the pene- two case.,+ are shown, The hardness, as a function of the
tration depth, in the hardness measurements, the penetra- ratio d/t, is drawn in Fig. IO. For the coated specimen,
tion depth is chosen rlol to exceed 10-20% of the film I'rorn d/t x 100 = 15G to d/t X I O0--35g+, the hardness
thickness in order lo avoid st~bstu'ate ct'l'ccts, In our sirnula- of T i N / H S S sy~:tcm with respect to bulk TiN decreases,
tit)n, wc have compared a bulk TiN specimen with a 2 Izm tlp to a I'qa,x i m u i l l deviation of 33~.
thick TiN coating on HS5 substrate The indenler pene- The analysis of the plastic field during the nanoindenta-
trated up to ().7 /zm, ct)rrcsrmnding to 35+;]+ of the rilm lion process indicates a correlation between the onset of
thickness, the substrate plastic deformation at the interface and the
Fig. 8 shows the rcsuhs of the numerical analysis Ior initial separation of tile loading curves. Fig. I i shows the
Ihe bulk TiN (open triangles) and for Ihe T i N / H S S system history el +the plastic deformation of the coated specimen.
(solid circles). At a value t)f perietnltion d equal to 15G of In order to be able to detect the beginning of the first
the I'ilm thickness t. the twu loading curves begin to relevant plastic defommtion in the substrate, we have
diverge. The curve of the coaled specimen changes ils chosen to refine the interval of the equivalent plastic strain
curvature and tile final penetn'ation is rcacl~ed for a 3(Y~ variable Lmder a threshold value of 4.E-2, In Fig, I la, the
smaller ioad than in Ihc case of the bulk malcrial. There- penetration depth is 13+,~+. of the t+ilm thickness. At this

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---~ d) b) c)

Fi#. I I. I!tluivak'nl I',ht.,.ti~. ',traim,: (a) rl/1 × I(X) = I?",: : (1',) +//l -"'. 10<1' = 15';+ the h.tlh'4rat,,.' Ix.'32iu~ to pla,,tif} al II1,.." iilletlaee i~,#io,, (L_.) ,d/t ~ IIHI = 19';
cnhtrgclllctlt ur the i'da,,{ificd region in the ,,ub,,trat,',
2414 M, Lichim'hi el . I . / Thin Snlhl Fihns 312 f 1~9,~') 240..248
stage ot" the indentation, only 'he film is plastically de-
forrned. At d / l = 0.15, the st, bsirale shows plastic defter-
motion at the interface whereas the coating does nol (see
Fig. lib). This is exactly the d / I value at which the
loading curve of the bulk TiN deviates from that of the
TiN coating. Fig. I Ic) shows an even larger plastic region
for d / t = 0.17. The three d / t values arm indicaled in Fig.
8.
5. Conclusions
in this work we have studied the Berkovich nanoinden-
ration process hy means of finite elemem analy,,,is, We
have verified thai an axisymmetric model gives the ~ame
results as a three-dimensional model if tl~e conical indenter
has the same area function as a Berkovich lip, Since Ihe
axisymmetric model has a lower numher of degrees of
freedom and, consequently, requires shorter conlpulaiional
time, it was used for all the analyses presellled. For leStill~
the fea.~ibilily of the model we compared e×perirnental
data of a nanoindentation measurcmenl performed on a
T i N / H S S specimen with numerical resulls. The loading-
unloading curves present good agreernenl, even if there is
a slight discrepancy in the loading section.
The effect of the suhsira~e siilTness on coaling hardness
measuremenls was analyzed for the T i N / H S S syslem
through lhe evolution of the plastic deformalion field. The
initiation of plastic defornlalion in Ihe Stlhslr;.ite at the
interface zone corresponds Io a pt,~nelr;llion depth of lhe
indenter equal Io 15~;~ of the film thickness. This relative
penetration of ll'ie inderlier repre~erils a critical point from
which the load d:lla begin to he affected by the lower
stiffness of lhe subsffate. Consequently, at lhis stage the
h-irdness ot" lhe t'ilm decreases with respect to the real
value. TI]us, Ihe gefieral criterion lhal the I'ilm should not
be penelraled nlol'e lhan 10-20cA of its Ihil.'kness is still
acceptable Ibi "FiN on ltSS.
Acknowledgements
The authors wish io thank W, Gissler and H. Sttinlnl for
helpful discussions, A. Hofftllililn and T. Siisaki for wiltl-
able t¢cllilical assislance. One of the authors is grateful to
the Lahoralorio Materiali innovaiivi ( L a M I ) o f the Univer-
sit), of Basilicala (Italy) and lo the RegiOlle Basiliclila t])r
Iheir financial support.
References
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[f>] I1.1:. WalIL~. H. Ii;ingCll. Malcr. S¢i. l'n~. Alfi (ItJq3).t4.t.
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