V ol. 16　 N o .

1 　　　　　　　　　　　　 CHIN ESE JO U RN A L OF A ERO N A U TICS 　　　　　　　　　　　　　　 February 2003

Hardness Measurement and Eval uation of Thin Film

on Material Surf ace
WANG L in-dong, L I Min, ZHANG T ai-hua, L IANG Nai-gang
( State K ey L ab. of N onlinear M echanics, I nstitut e of M echanics,
Chinese A cademy of Sciences , Beij ing 　100080, China)

Abstract: 　 A method for hardness measurement and evaluation of thin films on the material sur face
was proposed. F irstly , it is studied ho w to obt ain the fo rce-indentatio n response with a finite element
method w hen the indentation is less than 100 nano meter s, in which cur rent nanoindentation ex per i-
ments have not reliable accuracy. T he w hole hardness-indent ation curv e and fitted equation were ob-
tained. A t last, a formula to pr edict the hardness of the t hin film o n the material sur face was deriv ed
and favo rably compared with ex per iments .
Key words : 　 thin film material ; hardness; nanoindentation ; finite element simulation
材 料 表面 薄膜 硬度 的测 试 计算. 王 林栋 , 李　 敏, 张泰 华, 梁 乃刚. 中 国 航空 学报 ( 英文 版) .
2003, 16( 1) : 52- 58.
摘　要: 给出了 基于纳米硬 度试验的 表层薄膜的 硬度测算 方法。
首 先研究如 何利用有限 元计算弥
补纳米硬度测量在压痕深度小 于百纳米时的精度缺 陷, 进而探 讨薄膜- 基体材料 系统的硬度随压
痕深度变 化的规律, 最后导 出了根据 实验曲线预 测表层薄 膜材料的硬 度的公式, 并进行 了实验验
证。
关键词: 薄膜材料; 硬度; 纳米压痕; 有限元模拟
文章编号: 1000-9361( 2003) 01-0052-07　 　中图分类号: V 252; T G 113. 25 + 1　 　文献标识码: A

　　T o meet t he requirements of w ear -resist ance , ness of t hin film s can hardly be directly det ermined
corrosion-resistance and fatigue-resistance, t he t hroug h indent at ion because of t he precision limit a-
materials with a t hin f ilm on t he surf ace have at- tion of t he indentation equipment . In f act , t he
tract ed a g reat deal of at tent ion and have been hardness obt ained f rom ex periments shows t he
w idely used in many industrial fields such as aero- combined action of the thin film and substrate.
naut ics, astronaut ics, vessel and automobile eng i- T herefore, how to ev aluate the hardness of thin
neering, etc. For ex am ple, heat -resistance coat ing films becomes an important problem t o be over-
technology is adopted on t he blade of an aeroeng ine come urg ent ly.
[ 2-5]
in order t o im prove performance and increase it s A lot of lit erat ure have invest ig at ed t he
service life . In practice , how to obtain t he m e- measurement methods of hardness of thin f ilm m a-
chanical propert ies of t hin film materials is a gener- terials . In general, the “ 10 percent rule ”is a fun-
al problem and evaluating t he hardness w ith damental rule to evaluat e the hardness of thin
nanoindentation is a simple and ef fective m et hod to films; i. e. when t he depth of indentation is less
[ 1]
solve the problem . How ever , w it h the develop- t han 10% of t he thickness of a t hin f ilm, t he influ-
ment of science and t echnology , many advanced ence of t he subst rat e on the ex perimental result
requirements f or mat erials are broug ht forw ard and w ill be less t han 2% . T o som e ex tent , t he “10
2
many films w ith t hickness of t he order of 10 up to percent rule”is ef fective , but the met hod obvious-
[ 6]
10 nanom et ers are made. In t his case , the hard- ly has it s limit ations . When t he t hickness of t he
Received dat e: 2002-09-11; R evision received dat e: 2002-10-25
Foundation items: C hinese A cademy of Sciences Foundation ( KG CX 1-11) ; N at ional Nat ural S cience Foundat ion of China ( 10232050) ; M in-
ist ry of S cience and T ech nology Foundat ion( 2002CB412706)
A rt icle U RL: ht t p: / / ww w . hkx b. n et . cn/ cja/ 2003/ 01/ 0052/
© 1994-2010 China Academic Journal Electronic Publishing House. Open access under CC BY-NC-ND license. http://www.cnki.net
 Hardness M easurement an d Evaluat ion of Thin Film
February 2003 ・ 53・
on M at erial S urface

thin f ilm is less than 1 m, according t o the rule, depth of indentat ion, by w hich the boundary eff ect
the depth of indentation should be less t han 100nm can be neg lect ed. According t o sym met ry , 1/ 6 of
and the corresponding m easurement dat a should be t he indent er and f ilm/ substrat e composite is con-
reliable, which w ill be beyond the abilit y of t he sidered.
present experim ent technolog y .
From the point of view of mechanics , the pro-
cess of nanoindent ation is very complex . In t he
process, the m at erial in diff erent places under t he
indent er will undergo diff erent procedures and be
in different st ates, w hich is very diff icult t o handle
w it h an analyt ical met hod. Numerical simulat ion
has at t ract ed a great deal of att ention because of it s
distincted advant ages over t he analyt ical
[ 7] F ig . 1　 Shape and par amet er s of Berkovich indenter
method , w hich is not rest ricted by t he depth of
As show n in Fig. 2, a four-node-t et rahedron
indent at ion and can probably represent the w hole
process. elem ent is adopt ed . In order to g uarant ee calcula-

In t he present paper, t he geom et rical shape of tion precision and save calculat ion costs, t he mesh
is fined locally rather than globally in t he present
the indenter is precisely simulat ed and the process
of nanoindentation is analyzed w ith a t hree-dimen- finit e element model. F or inst ance, t he size of t he

sional finite element method ( F EM ) . T he loading mesh in t he contact region is smaller than t hat of
t he mesh in ot her regions.
and unloading processes of t he indent ation ex peri-
ment , as w ell as the hardness-displacement curve
of nanoindentation are represent ed t hrough t he
variation of the mesh scale. For f ilm/ substrat e
composite , the reg ularity of hardness t o indent a-
tion depth is discussed . T he fit ting hardness for-
mulae by which the hardness of thin f ilm mat erials
can be predicted according to the ex periment al
curv es are proposed and verified by experiment s.

1　Sim ulation of Nanoindentation

In the present w ork, a t hree-dimensional f i- Fig . 2　 Finite elem ent model

nite element model and Berkovich t riple pyramid 1. 2　Characteristics of material

indent er w it h t he t ip radius less than 100 nm are
adopted. T he loading and unloading process w ith
gliding cont act can be simulated .
[ 8]
1. 1　Geometrical shape and mesh
As show n in Fig . 1, Berkovich indent er, t he
standard indenter of nanoindent ation equipment ,
has a geom etrical shape of a t riple pyram id and t he
heig ht is set t o be 3 m . T he w hole material is di-
vided int o t wo parts, i. e. , thin film and sub-
strate. In t he present model, the size of t he m at e-
rial is assumed t o be 25 times greater t han t he
© 1994-2010 China Academic Journal Electronic Publishing House. Open access under CC BY-NC-ND license. http://www.cnki.net
T he indent er should be handled as an elastic
body because the hardness of the indenter and that
of t he f ilm/ substrat e may be of the same order . In
t his paper , t he Young' s modulus of t he indent er is
set t o be 1141GP a and t he specimen is modeled as
a von Mises solid w it h discret e yielding follow ed by
linear, isotropic work hardening. P ropert ies of t he
material of t he specimen are show n in F ig . 3, in
w hich E is Young ' s modulus, Y is yield streng th,
and E T denot es hardening modulus.
T he hardness of the f ilm/ subst rat e composit e
 ・ 54・ W A N G Lin-dong , LI M in, ZHA NG Tai-hua, LIAN G N ai-gang CJA

Fig. 3　 Stress-strain cur ve of mater ial Fig. 4　Comparison o f FEM and ex per imental result s
w ill vary w it h the dept h of indent at ion because t he 　　FEM m esh scale can be controlled and then
properties of the film and subst rat e are diff erent . t he hardness of t he mat erial can be calculat ed for
T o invest ig at e the reg ularity of mat erial hardness, nanoindentation . In general, t he f init e elem ent
it is the key point to analyze t he inf luence of char- analysis is not af fect ed by t he absolute size of t he
acterist ic dif ference betw een t he film and the sub- mesh, and the advant ag e is t aken to investigate t he
strate on t he variat ion of hardness w ith the inden- variation of hardness when the depth of indent a-
tation depth. T he influence is invest ig at ed through tion is less t han 200nm in the present st udy .
parameter combinat ions of the f ilm and the sub-
strate as show n in T able 1. In the t able , Y f and Y s 2　Regularit y of Hardness Variation of
are y ield streng th, E f and E s denote Young 's mod- Film w ith Indentation Depth
ulus, v f and v s are Poisson' ratio, and E T f and E T s
Som et imes, the thickness of a t hin film is on-
represent hardening modulus, w here subscripts “ f” 2
ly of t he order 10 up t o 10 nanometers. In t his
and “
s”stand f or f ilm and subst rat e respectively.
case, the real hardness of t he f ilm can be obt ained
Table 1　Yiel d strength ratios and Young' s modul us
ratios of f il m to substrate in models
only w hen t he dept h of indentation is very small.
Yield st rengt hs
Conf ined by t he precision of the present indent a-
10 20 50 200 500 1000 1500 3000
of f ilms Y f / M Pa tion, t he hardness of the material cannot precisely
Yf/ Ys 0. 1 0. 2 0. 5 2. 0 5. 0 10. 0 15. 0 30. 0
Y oung' s m oduli
be det ermined w hen t he dept h of indent at ion is less
25. 6 64 256 384 640
of f ilms E f / GPa t han 200nm , especially 100nm .
Ef / Es 0. 2 0. 5 2. 0 3. 0 5. 0
Fig . 5 show s the hardness-displacem ent curves
( Y s = 100M Pa, E s = 128G Pa, vf = vs = 0. 3, E Tf = E T s = 2. 6G Pa)
obt ained by indent at ion for T i/ Si mat erial. It can
1. 3　Experimental verification of FEM resul ts
be seen t hat all the curves f luctuat e severely when
T o verif y the reliability of t he f init e element
t he dept h of indent at ion is less than 150nm . T his
model, T i/ Si material, a ty pical sof t f ilm on hard
substrate , is select ed as ex periment al material of
nanoindentation. For t he mat erial, t he hardness of
the f ilm is approximately equal to 1/ 3 of that of
the subst rate . T he comparison of F EM and ex peri-
mental results is show n in Fig. 4, w hich indicat es
that the result s calculat ed by t he present m odel are
ex cellently in good ag reem ent wit h the ex perimen-
tal ones. In addit ion , many t imes of experim ent s
are done and t he result s show good repeatabilit y.
T o be clear , only tw o experim ent al curves are g iv- F ig . 5　 T he har dness -displacem ent cur ves o btained by
indentation for T i/ Si material
en in Fig . 4.
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 Hardness M easurement an d Evaluat ion of Thin Film
February 2003
on M at erial S urface
indicates t hat the hardness of t he thin film cannot
be obt ained by ex periment .
T o investigate the relat ionship of the hardness
of t he composit e w it h that of the film and sub-
strate , mat erial models of the com posit e, film and
substrate are independently est ablished to calculat e
their hardness respectively. F ig . 6 giv es t he hard-
ness-displacement curves, in w hich curv e 1 reflect s
the film , curve 2 represents t he com posit e, and
curv e 3 denot es the substrat e. It can be seen that
curv es 1 and 3 vary flat ly and st raightly, w hich is
[ 9]
in accordance w ith the prev ious research . Curve
2 locat es betw een curve 1 and curve 3, and it
matches curve 1 f or small indent at ion because t he
hardness is mainly det ermined by t he f ilm rat her
than by the subst rate .
F ig . 6　T he har dness-displacement curves
obtained with FEM
3　Hardness Evaluation of F ilm M aterial
When t he t hickness of t he film is less than
1 m, the hardness cannot precisely be det ermined
by nanoindent at ion . In the present w ork, t he
load-displacement curve of nanoindent ation is sim-
ulat ed w it h FEM , and t he main f actors t hat aff ect
hardness are investigat ed . A hardness formula , by
w hich t he hardness of t hin film material can be
predicted according t o the experim ents, is derived
by invest igat ing a great deal of data of f ilm / sub-
strate com posit es.
3. 1　Infl uences of material parameters on
resul ts
T he load-hardness curve by w hich t he m e-
chanical propert ies of m at erial can be represent ed is
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・ 55・
t he basic result of indent ation. In this paper, t he
influences on the results of the yield streng th ,
Young ' s modulus, hardening modulus and
Poisson' s ratio of t he film are analyzed and t he
main paramet ers are determined .
Diff erent load -displacement curves can be ob-
tained by changing t he yield strengt h rat io of f ilm
t o subst rat e show n in T able 1. Fig . 7 gives t he
curves w hen t he yield strengt h ratio Y f / Ys
changes. It can be seen t hat t he y ield st reng th ra-
tio is a smart param et er that makes influence on
t he loading process.
Fig. 7　L oad-displacement cur ves of different
y ield strength r atio
T he influence of the yield st rengt h and
Young ' s m odulus of t he film on the loading curve
is show n in F ig . 8. It can be seen t hat t he inf luence
of Young' s m odulus is f ar less t han t hat of t he
yield st rengt h w hen t he thickness of t he f ilm is
small. In t his case, t he influence of Young 's mod-
ulus on t he results can be neglect ed.
Hardening moduli of many mat erials are far
less t han their Young' s m oduli, and t he rat io is set
t o 0. 0- 0. 1 in t he present w ork. F ig . 9 shows t he
Fig. 8　 Compar iso n o f influence o n load -displacement
cur ves of Y oung 's modulus and yield st reng th
 ・ 56・ W A N G Lin-dong , LI M in, ZHA NG Tai-hua, LIAN G N ai-gang CJA

influence of t he hardening m odulus rat io of the f ilm

to the substrate on t he results. As show n in t he
figure, t he inf luence of the hardening modulus of
the f ilm on t he loading curve is insig nificant .
When t he hardening modulus of t he film increases
by 5 t im es, t he variance corresponding t o t he max-
imum displacement is no m ore t han 10% . T here-
fore, t he inf luence of the hardness modulus on the
result s is neglected in t his paper .
Fig. 10( a) 　 T he fitting cur ve w hen Y f / Y s is 5 1

Fig. 9　L oad-displacement cur ves of different

hardening modulus r atio F ig . 10( b) 　T he fitting cur ve w hen Y f / Ys is 10 1
In addition, previous research indicat ed that
the inf luence of Poisson' rat io on t he result s is very
small, which is verif ied by the present w ork. In
view of t his, t he inf luence of Poisson' rat io is also
neglect ed in the present analysis.
3. 2　Fitting formul a of hardness-displ acement
curves
As m entioned above , t he hardness of a thin
film cannot be direct ly obt ained through indent a-
tion because of t he lim it at ions of experiment al pre-
Fig. 10( c) 　 T he fit ting cur ve when Y f / Y s is 1 5
cision, so an ef fective met hod t hat can det erm ine
the hardness according to hardness t est s is t o be H = H s + ( H f - H s ) exp[ - h/ t ] ( 1)
derived. In this paper, how t o figure out the hard- w here H f and H s are hardness of t he film and sub-
ness of a thin f ilm by f it ting t he hardness-displace- strate, and h and t are t he dept h of indent at ion and
ment curve of the film / subst rate composite accord- t he t hickness of the film , respect ively . H is t he
ing t o t he experim ent al data w hen the depth of in- measured hardness w hile t he dept h of indent ation
dent at ion is large enoug h is invest ig at ed. is h.
Figs. 10( a) , ( b) and ( c) are t he fit ting hard- As show n in Fig . 10, H w ill tend to H f when
ness-displacem ent curves of t he film / substrate . h approaches 0, i . e. the hardness calculat ed by
T he dat a required t o be acquired f rom indent at ion Eq. ( 1) w ill approach t he hardness of the f ilm a-
and the data provided by FEM are show n in t he long w ith t he reduction of the indent at ion dept h .
figures. 3. 3　Hardness of fil m
By f it ting the result s obt ained t hroug h a great In Eq . ( 1) , let = 2. 2. T hen
deal of param et er combinations, t here is H = H s + ( H f - H s ) ex p[ - 2. 2h/ t] ( 2)
© 1994-2010 China Academic Journal Electronic Publishing House. Open access under CC BY-NC-ND license. http://www.cnki.net
 Hardness M easurement an d Evaluat ion of Thin Film
February 2003
on M at erial S urface
From Eq. ( 2)
H f = H s + ( H - H s) exp( 2. 2h/ t)
Eq. ( 3) is t he f ormula t o calculate t he hardness of
the f ilm . As long as t he parameters t, H s and H
are m easured by experiment, t he hardness H f of
the film w ill be known.
T o reduce error , m ult i-point m easurement
should be follow ed and m ake t he mean value as t he
final result . Assume N t imes of m easurement are
done. According t o Eq. ( 3) , there is
N
1 specim en . T he hardness of t he t hick f ilm T i direct-
N∑
Hf= Hs+ ( H n - H s) exp( 2. 2hn/ t )
n= 1
( 4)
w here hn is t he depth of nth indentation, and H n is
the corresponding hardness. In order t o improve
prediction precision , more than 5 points wit hin t he
scope of 0. 2t< h n< 1. 2t should be selected.
4　Ex perimental Verification
For f ilm/ substrat e composit es, as discussed
above, Eq. ( 4) can give t he hardness of t he f ilm
w hen t he f ilm t hickness t , substrate hardness H s
are know n and the nanoindentation curve is ac-
quired from ex periment . In t he present w ork , ex-
periment s are done to verif y Eq. ( 4) . In t he ex per-
iment s, t ypical T i/ Si materials are select ed as t he
specim ens , and the thickness t of T i f ilm is
200nm . According t o indentation, t he hardness
H s of t he substrate is 10. 5GPa . Fig . 11 g ives t he
hardness-displacement curve obtained with ex peri-
ment .
As show n in Fig. 11, t he hardness of t he
specim en gradually f alls along w it h t he reduct ion of
the indentation dept h, which indicat es t hat t he
F ig . 11　Hardness-displacement curve of T i/ Si
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・ 57・
specim en is a sof t f ilm on a hard substrate. T he
( 3) hardness of t he film cannot be det ermined by ex-
periment because t he thickness of t he film is only
200nm . In f act, t he hardness obt ained from ex-
periment s show s t he combined action of t he thin
film and substrat e.
According t o Eq . ( 4) , the hardness H f of thin
film T i is 3. 68GPa. In order to direct ly obt ain t he
hardness of f ilm T i w ith indent at ion, a T i/ Si com-
posit e w it h a t hick film is then select ed as anot her
ly g iven by nanoindentation is 4. 10GPa . T he rela-
tive error of the hardness calculat ed by Eq. ( 4) to
t he experim ental result is less than 10% , w hich
indicates that the present met hod is ef fect ive for
film / substrate com posit es.
5　Conclusions
( 1) F or f ilm / subst rat e com posit es, t he hard-
ness-displacem ent curve of nanoindent at ion can be
sim ulat ed by FEM , w hich overcomes the precision
limitat ions of nanoindent at ion w hen the indent a-
tion depth is less than 100nm.
( 2) Based on t he nanoindent at ion, t he hard-
ness of a t hin film on the substrate can be eff ective-
ly obt ained from Eq. ( 4) .
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Biography:
Wang Lin-dong　Born in N ov . , 1976,
he is pursuing his M aster degr ee in the
State Key Lab of N onlinear M echanics,
Institute of M echanics, Chinese A cade-
my of Sciences. E-mail: w ang ld @ lnm .
imech. ac. cn

© 1994-2010 China Academic Journal Electronic Publishing House. Open access under CC BY-NC-ND license. http://www.cnki.net