Surface and Coatings Technology 154 (2002) 304313

Relationships between hardness, Youngs modulus and elastic recovery in

hard nanocomposite coatings

J. Musil*, F. Kunc, H. Zeman, H. Polakova

Czech Republic
Department of Physics, University of West Bohemia, P.O. Box 314, 306 14 Plzen,
Received 19 November 2001; accepted in revised form 11 December 2001

Abstract
The paper is devoted to an assessment of the mechanical behavior of hard and superhard nanocomposite coatings from loadingy
unloading curves measured by a computer-controlled Fischerscope H 100 microhardness tester and a maximum depth dmax of the
diamond indenter impression into the coating at a given load L. It is shown that: (1) the area between the loadingyunloading
curve and the value of dmax decreases with increasing (i) hardness H, (ii) effective Youngs modulus E *sEy(1yn2 ) and (iii)
universal hardness HU, where E and n are the Youngs modulus and the Poisson ratio, respectively; and (2) there is no simple
relation between the mechanical response of the coating and H or E * alone; however, this response is strongly dependent on the
ratio HyE *. The last fact gives a possibility of tailoring the mechanical properties of a coating for a given application, e.g. to
prepare coatings with high hardness H, high resistance to plastic deformation (;H3 yE*2 ), high elastic recovery We , but with low
E * and high dmax. Special attention is also given to the analysis of problems in accurately measuring the hardness of superhard
(G60 GPa) coatings. It is shown that a high elastic recovery We G80% of superhard films with HG60 GPa (1) strongly decreases
the gradient dHydL and (2) shifts the region L, where H(L)fconstant and the hardness H is correctly measured, to higher values
of L. This means that the lowest load L used in the hardness measurement must be higher than L used in measurements of
coatings with H-60 GPa to prevent the value of H measured from being significantly higher than the real hardness of the
coating. 2002 Elsevier Science B.V. All rights reserved.
Keywords: Nanocomposite films; Mechanical properties; Microindentation measurements; Magnetron sputtering

1. Introduction
It is well known that the properties of every material
are closely connected to its structure. The structure,
however, depends on the phase and chemical composition of the material, and this in turn is strongly dependent on the preparation method. Therefore, the
development of new materials becomes a complex and
difficult task. First, the relationship between the structure
of the material and the conditions of its preparation
must be found; this argument is particularly valid for
materials produced in the form of coatings. Increasingly,
thin-film coating techniques are being used as a flexible
method to produce new materialsmany of which
cannot yet be synthesized by conventional methods.
*Corresponding author. Tel.: q420-19-7423136; fax: q420-197422825.
E-mail address: musil@kfy.zcu.cz (J. Musil).

Hard materials are currently characterized by their

hardness, H, effective Youngs modulus E *sEy(1yn2)
and elastic recovery We, where E and n are the Youngs
modulus and the Poisson ratio, respectively. For hard
coatings, these quantities can easily be determined from
loadingyunloading curves measured by nanoindentation
or instrumented microhardness testing. Recently, for
instance, such measurements were used to characterize
the macrostresses generated in CNx films during deposition by reactive magnetron sputtering of a graphite
target in pure nitrogen discharge w1x. Here, it was shown
that stresses in CNx films deposited onto a Si(001)
substrate can be directly correlated with the film microstructure (low stresses for an underdense columnar structure and high stresses for a dense, distorted
turbostratic-like cross-linked microstructure) and particularly that We increases, and maximum penetration depth
dmax of the diamond indenter decreases, with increasing
H (and vice versa). Similar experimental results have

0257-8972/02/$ - see front matter 2002 Elsevier Science B.V. All rights reserved.
PII: S 0 2 5 7 - 8 9 7 2 0 1 . 0 1 7 1 4 - 5

J. Musil et al. / Surface and Coatings Technology 154 (2002) 304313

305

The article deals with (i) a systematic investigation

of the loadingyunloading curves of different nanocomposite coatings prepared by magnetron sputtering, (ii)
correlations between H, E * and We and (iii) the effect
of H and E * on the resistance of materials to plastic
deformation.
2. Experimental details

Fig. 1. Typical indentation loaddisplacement curve measured using

a microhardness tester. Areas I and II represent plastic deformation
and elastic recovery, respectively.

also been reported by Karlsson et al. w2x. They showed

that for arc-evaporated TiC0.15N0.85 films, the value of
dmax decreases with both increasing stress s and H. On
the contrary, Matthews and Leyland w3x discussed the
importance of the elastic modulus E and the ratio HyE
in determining the endurance capability of a surface
coating, especially its ability to accommodate substrate
deflections under load.
Recent experiments, however, have shown that hard
nanocomposite coatings with the same hardness can,
according to their chemical composition, exhibit different values of the effective Youngs modulus E * w4,5x.
This means that there is a possibility of tailoring the
mechanical properties of a material for a given application, but there is no simple relationship between all
three quantities, H, E * and We, that characterizes this
mechanical behavior. Therefore, it is necessary to find
some general relationships between H, E * and We. This
task is the main subject of the article.

All hard and superhard nanocomposite coatings

reported in this article were prepared by DC reactive
sputtering using an unbalanced magnetron equipped with
alloyed or composite targets with a diameter of 100
mm.
The nanocomposite coatings were characterized using
a computer-controlled Fischerscope H 100 microhardness tester equipped with a Vickers diamond indenter.
The hardness H and universal hardness HU measured
by this instrument are defined by the following formulae
w6,7x:
HsLmaxy26.43dcor.2

(1)

HUsLmaxy26.43dmax.2

(2)

where the diamond indenter penetration depths dcor and

dmax are defined in Fig. 1. The hardness H is determined
from the plastic component of the coating deformation
only. On the contrary, the universal hardness HU is
determined by both plastic and elastic components of
the coating deformation. Therefore, the value of HU is
lower than the value of H. Each hardness value was
determined as a result of 10 indentation tests.
The typical thickness of the coatings is approximately
4 mm. This ensures that all coatings fulfil the criterion
dyhF0.1, which guarantees that measurement of the
hardness is not significantly influenced by the substrate,
where d and h are the depth of the diamond indenter
impression into the coating and the thickness of the
coating, respectively.
3. Loadingyunloading curves

Fig. 2. The loadingyunloading curves of the hard (13 GPa) and superhard (46 GPa) CrNiN nanocomposite coatings.

The evaluation of microhardness, H, effective Youngs

modulus E *sEy(1yn2) and elastic recovery We from
the loadingyunloading curves measured by an instrumented microhardness tester is a standard methodology
used for the characterization of coating materials. A
typical loadingyunloading curve is shown in Fig. 1. The
area between the loading and unloading curve represents
the energy dissipated in the coating due to plastic
deformation, and the area under the unloading curve
represents the elastic energy for deformation. From
measured values of H and E *, it is easy to calculate the
ratio H 3 yE *2, which is proportional to the resistance of
the coating to plastic deformation w8x. This essentially
means that the higher the resistance to plastic deformation, the higher is the ratio H 3 yE *2. In general therefore,

J. Musil et al. / Surface and Coatings Technology 154 (2002) 304313

306

Table 1
Mechanical parameters of hard (12.7 GPa) and superhard (46 GPa)
CrNiN films measured at the diamond indenter load Ls20 mN
H
wGPax

E*
wGPax

We
w% x

HU
wGPax

H 3yE *2
wGPax

HyE *
wmmx

dmax

12.7
46.0

273
352

35
71

7.9
14.0

0.03
0.78

0.05
0.13

0.31
0.23

Table 2
Mechanical parameters of films with approximately the same hardness
H and different values of E * measured at the diamond indenter load
Ls20 mN

Table 3
Mechanical parameters of films with the same resistance to plastic
deformation, i.e. H 3yE *2fconstant measured at the diamond indenter
load Ls20 mN
Film

H
wGPax

E*
wGPax

We
w% x

HU
wGPax

H 3yE *2
wGPax

HyE *

dmax
wmmx

CrNiN
CrNiN
TiMoN

31.8
34.5
44.5

253
287
401

74
75
77

10.7
11.8
15.1

0.50
0.50
0.55

0.126
0.120
0.110

0.267
0.254
0.224

Film

H
wGPax

E*
wGPax

We
w% x

HU
wGPax

H 3yE *2
wGPax

HyE *

dmax
wmmx

ZrYN
ZrYN

31.6
32.1

229
296

80.3
73.4

9.9
11.9

0.60
0.38

0.137
0.108

0.195
0.178

CrNiN
TiMoN

39.2
43

307
442

74
68

12.6
15.9

0.64
0.41

0.128
0.097

0.246
0.218

imum depth dmax of the diamond indenter penetration

into the film decreases with increasing H of the film.
Moreover, from Table 1 it is evident that the CrNiN
film with a higher hardness (46 GPa) exhibits higher
values of E *, We, H 3 yE *2 and HU. This is the main
difference in the mechanical response of the hard and
superhard films to the diamond impression into their
surface.

AlCuN
TiMoN

47
46

313
413

84
75

12.9
15.5

1.06
0.57

0.15
0.11

0.24
0.22

3.2. Effect of Youngs modulus E

a low E * becomes desirable, as it allows the given load

to be distributed over a wider area. This argument
(although valid) is in contradiction to conventional
linear-elastic fracture mechanics theory, which predicates
a high modulus (to prevent crack growth) for tough
materials.
3.1. Effect of hardness H
The effect of coating hardness H on the loadingy
unloading curves is shown in Fig. 2, with typical
loadingyunloading curves measured for soft (12.7 GPa)
and superhard (46 GPa) coatings. Fig. 2 compares two
CrNiN nanocomposite films, prepared under different
deposition conditions, the mechanical quantities of
which are summarized in Table 1. As expected, the area
between the loading and unloading curve and the max-

There is no simple relation between the film hardness

H and its effective Youngs modulus E *. Experiments
show that it is possible to produce films with the same
hardness H and different values of E *; see Table 2. This
means that films with the same hardness can exhibit
different resistance to plastic deformation. The effect of
different values of E * on the loadingyunloading curves
at the same (i) hardness H and (ii) resistance to plastic
deformation H 3 yE *2 is shown in Fig. 3a,b. Mechanical
quantities characterizing the films that exhibit the same
resistance to plastic deformation are summarized in
Table 3.
From Fig. 3a and Table 2, it is clearly evident that an
increase in E * results in (a) a decrease in We, H 3 yE *2
and dmax, and (b) an increase in HU. For films with the
same resistance to plastic deformation (Fig. 3b and
Table 3) the value We, however, slightly increases with
increasing E *. This is due to the fact that with increasing

Fig. 3. Effect of increasing effective Youngs modulus E * on the maximum depth dmax of the diamond indenter impression for (a) films with the
same hardness H of approximately 46 GPa and (b) films with the same resistance to plastic deformation (H 3yE *2f0.5 GPa).

J. Musil et al. / Surface and Coatings Technology 154 (2002) 304313

Fig. 4. The dependence of the film hardness H as a function of effective Youngs modulus E * for selected hard nanocomposite and binary
nitride films magnetron-sputtered under different deposition conditions w4,5x.

E *, the hardness H increases and the ratio HyE * decreases. This experiment clearly shows that the mechanical
behavior of a hard film strongly depends on the combination of its hardness H and effective Youngs modulus E *.
Recent experiments show that the relationship
between hardness H and effective elastic modulus E * in
the hard film can be controlled by the choice of (i) its
chemical composition (see Fig. 4) and (ii) the deposition parameters used for its formation (see for instance
w4,5,9x). Fig. 4 gives experimental evidence that the
production of films exhibiting the same hardness H and
different values of E * is possible. This means that, in
principle, it is possible to tailor films with prescribed
mechanical properties for a given application.

307

Fig. 6. The loadingyunloading curves of two TiAlVN films exhibiting the same hardness H and different values of elastic recovery
We, and one TiAlVN film with low H (11 GPa), low We (41%)
and high plastic deformation, i.e. low H 3yE *2 ratio.

3.3. Effect of elastic recovery We

3.3.1. Films with different H and the same We
In general, the effective Youngs modulus E * increases with increasing hardness H. This is the simplest
situation. In this case, the resistance to plastic deformation H 3 yE *2 increases with increasing H because the
ratio HyE * is approximately constant (Table 4). The
same ratio HyE * approximately correlates with the same
elastic recovery We. On the contrary, as can be expected,
the maximum indentation depth dmax decreases with
increasing H. Typical loadingyunloading curves of two
TiAlVN films with different hardness values H and
the same elastic recovery We are given in Fig. 5.
Table 4 shows that the films with the same elastic
recovery We can exhibit a very different resistance to
plastic deformation characterized by the ratio H 3 yE *2.
The harder the film, the higher is E * and the higher is
the resistance to plastic deformation.
The most important finding that follows from the
experiment described above is the fact that hard nanocomposite coatings with very different hardness can
even exhibit the same elastic recovery We, provided that
the ratio HyE * is approximately constant.
Table 4
Mechanical parameters of two TiAlVN films with the same elastic recovery We measured at the diamond indenter load Ls20 mN

Fig. 5. The loadingyunloading curves of two TiAlVN films exhibiting different hardness H and the same elastic recovery We.

H
wGPax

E*
wGPax

We
w% x

HU
wGPax

H 3yE *2
wGPax

HyE *

dmax
wmmx

26.0
45.6

233
405

71
72

9.7
15.4

0.32
0.58

0.112
0.113

0.28
0.22

308

J. Musil et al. / Surface and Coatings Technology 154 (2002) 304313

Fig. 8. Microhardness H of 2.4-mm-thick TiAlN, 4-mm-thick Ti

B and 6-mm-thick ZrCuN films magnetron-sputtered on 15330
CSN steel substrate as a function of the diamond indenter load L.

Fig. 7. Micrographs of the diamond indenter impressions into superhard AlCuN and ZrCuN films sputter-deposited on steel substrates under different loads ranging from 200 to 1000 mN.

3.3.2. Films with different We and the same H

The loadingyunloading curves of two TiAlVN
films with the same hardness (Hf37 GPa; see Table 5)
and different values of We are given in Fig. 6. For
comparison, the loadingyunloading curves for a soft
film with Hs11 GPa is also given in Fig. 6. This
experiment shows that the film with lower E * (250
GPa) exhibits (i) smaller area between the loading and
unloading curves and (ii) greater dmax and higher ratio
H 3 yE *2 and (iii) lower values of HU compared with
the films with higher E * (399 GPa), see Table 5.
From this experiment two important conclusions can
be drawn:
1. Hard films with the same (plastic) indentation hardness Hf37 GPa can exhibit very different values of
universal hardness HU. The value of HU is greater
for the film with the greater value of E *. This is due
to the difference in the method of H and HU
evaluation. The hardness H is evaluated from the

plastic deformation only). On the contrary, in evaluation of the HU, both plastic and elastic deformations
are considered. This means that the accuracy of H
determination will decrease with increasing We, and
more reliable hardness values of films with high
elastic recovery We)70% will be given by the
universal hardness HU values and not by H.
2. The hard film (Hf37 GPa) with high elastic recovery (Wef80%) (i) allows deeper penetration of the
diamond indenter tip compared with the film that
exhibits a lower We (63%) and (ii) therefore exhibits
a higher resistance to plastic deformation (Table 5).
This experiment shows the possibility of creating
new, very elastic, hard materials. On the other hand,
deeper penetration of the diamond indenter into the
hard elastic film can complicate the evaluation of its
toughness from cracks formed under higher indenter
loads L.
In addition, there may be an elastic contribution from
the substrate to the HU values measured (even at dy
hF0.1), which might not influence H, but could influence the HU value measured. It could be envisaged in
some circumstances that H would be too high (due to
elastic recovery of the coating) and HU too low (due
to elastic contribution from the lower modulus subTable 5
Mechanical parameters of three TiAlVN films, the loadingyunloading curves of which are displayed in Fig. 6, measured at
the diamond indenter load Ls20 mN
Film

H
E*
We HU
H 3yE *2 HyE * dmax
wGPax wGPax w%x wGPax wGPax
wmmx

TiAlVN 11
TiAlVN 38
TiAlVN 36

238
250
399

41
81
63

6.8
10.7
14.5

0.023
0.878
0.296

0.046
0.152
0.090

0.342
0.266
0.229

J. Musil et al. / Surface and Coatings Technology 154 (2002) 304313

309

indenter impressions in the surface of the films tested

under different values of L.
Superhard films with high ()60%) elastic recovery
We exhibit quite unique, and at first sight, unexpected
behavior. Fig. 7 displays diamond indenter impressions
into 3-mm-thick superhard AlCuN and ZrCuN
films created under different loads ranging from 200 to
1000 mN. The mechanical parameters of these films
measured at Ls20 mN are summarized in Table 6.
From Fig. 7, it is evident that (i) the high loads L)400
and )600 mN for the AlCuN and ZrCuN film,
respectively, are necessary to generate cracks in the film
and (ii) no radial, but only circular cracks are created
(a similar deformation mechanism is reported in w10x).
A lower value of L, which is sufficient to generate a
circular crack in the AlCuN film, can easily be
explained by greater penetration of the diamond indenter
tip into the film surface (see Table 6). The maximum
penetration depth dmax decreases with increasing HU or
H (Figs. 3 and 6 and Tables 3 and 5). Therefore, lower
dmax into the ZrCuN film results in higher L, compared to the AlCuN film, necessary to generate a
circular crack.
This experiment clearly indicates that generation of
the crack in the film is not sufficient to evaluate the
film toughness. The formation of cracks depends not
only on the diamond indenter load L, but also on (i)
the mechanical behavior of the film (HU, E *, H 3 yE *2),
(ii) the stress andyor adhesion state of the coatingy

Fig. 9. Dependence of the hardness H and the ratio dyh of the indenter
impression depth d and the film thickness h for 4-mm-thick TiB film
magnetron-sputtered from TiB2 target at: magnetron current Ids1 A;
substrate bias Ussy50 V; substrate ion current density iss1
mAycm2; substrate temperature Ts s550 8C; and argon pressure pArs
pTs0.6 Pa.

strate). Thus, the true hardness value would lie somewhere between H and HU.
4. Micrographs of diamond indenter impressions
It is claimed that the fracture toughness of films can
be determined from the measured dependence of the
length of radial cracks on the applied diamond indenter
load L w10x. We therefore created a series of diamond

Fig. 10. The dependence Hs f (L) for 7-mm-thick TiB film and HUs f (H) for two 4-mm- and 7-mm-thick TiB films, measured under different
values of L, magnetron-sputtered at: Ids1 A; Ussy50 V; iss1 mAycm2; Tss550 8C; and pArs0.6 Pa, from a TiB2 target.
Table 6
Mechanical parameters of superhard AlCuN and ZrCuN nanocomposite films magnetron sputtered on steel substrates and measured at the
diamond indenter load Ls20 mN
Film

H
wGPax

HU
wGPax

E*
wGPax

We
w% x

H 3yE *2
wGPax

HyE *
wmmx

h
wmmx

dmax
wmmx

AlCuN
ZrCuN

47
56

12.55
15.38

313
399

84
81

1.06
1.08

0.150
0.140

3.3
3.0

0.242
0.220

310

J. Musil et al. / Surface and Coatings Technology 154 (2002) 304313

Fig. 11. The dependence HUs f (H) and HUs f (We ) for TiB and AlSiCuN films magnetron-sputtered from a TiB2 target and a composite
AlSiCu wAlSi (90y10 at.%) alloyed target with a Cu fixing ringx target, respectively.

substrate interface (i.e. the propensity for film delamination) and (iii) the mechanical behavior of the
substrate. The accurate determination of film toughness,
therefore, still remains an open problem.
5. Correctness of measurement of the quantifiable
mechanical properties of hard and superhard
coatings
The basic mechanical properties of hard and superhard
coatings, i.e. the microhardness H, effective Youngs
modulus E * and elastic recovery We, are evaluated from
loadingyunloading curves measured by nanoindentation
or instrumented microhardness testing. The determination of these quantities for thin films is, however,
difficult because they vary strongly with the diamond
indenter load L used in their measurement. To obtain
real values of H, E * and We, the load L has to be
correctly chosen.

The correct value of the microhardness H is that value

which (1) does not depend on L and (2) is not affected
by the substrate. Therefore, too low values of L at
which H strongly varies with increasing L (due to
problems with determination of the true contact area
between the indentor and surface of its impression) and
too high values of L at which the ratio of the indenter
depth d and the film thickness h is greater than a
maximum value wusually (dyh)maxs0.1 is recommended
not to be exceeded for plastic hardness of hard coatings
on, say, tool steel, cemented carbides substrates and
silicon wafersx, cannot be used in determination of the
correct value H. This means that there is a certain
interval of L in which the measured hardness
H(L)fconstant and only the value H within this interval
for L is a correct value of the hardness of the film
measured.
For films with hardness HF50 GPa, the decrease in
H with increasing L from Ls0 is very steep, and the

J. Musil et al. / Surface and Coatings Technology 154 (2002) 304313

311

Fig. 12. H as a function of E *sEy(1yn2) for TiSiN, ZrYN,

ZrCuN and TiMoN nanocomposite films sputtered at different
deposition conditions, i.e. Ts, Us, is and pN2. H was measured at an
indenter load of 20 mN.

interval L for which H(L)fconstant is already reached

for relatively small values of L. In this case, a relatively
low load of Ls20 mN lies in the interval where H
almost does not depend on L and the correct value of
the film hardness Hcorrect is measured. A maximum
Lmax value that gives the correct value of Hcorrect is
limited by the ratio dyhs0.1, and this is higher for
increasing thickness of the film; see the ZrCuN film
in Fig. 8.
A completely different situation occurs in the case
where superhard films with hardness H)50 GPa are
measured; see the dependence H(L) for 4-mm-thick Ti
B film given in Fig. 8. For a superhard TiB film, the
hardness H very slowly decreases with increasing L, and
a much higher (G50 mN) load L has to be used to
reach the interval of L where H(L)fconstant. In this
case, the interval L ranges from approximately 50 to
150 mN. The corresponding interval of the ratio dyh
also shifts to higher values and ranges from approximately 0.08 to 0.15; see Fig. 9. This means that correct
measurement of the mechanical behavior of hard films
with high hardness above 60 GPa, which always exhibit
high elastic recovery WeG70%, has to be carried out at
higher ratios of dyh (up to approx. 0.15) compared to
those allowed in the measurement of hard films with
H-50 GPa, i.e. when a maximum value of the ratio
(dyh)maxs0.1 should not be overcome. This finding is
of fundamental importance. The hardness of superhard
()60 GPa) films Hmeas. measured at L-50 mN is
higher than the correct value of the hardness Hcorrect of
the film measured, i.e. Hmeas.)Hcorrect.
5.1. Universal hardness
The hardness H of the film is determined from a
plastic component of the film deformation induced by

Fig. 13. We as a function of (a) H, (b) E *sEy(1yn2) and (c)

H 3yE *2 for TiSiN, ZrYN, ZrCuN and TiMoN nanocomposite films sputtered at different deposition conditions, i.e. Ts, Us,
is and pN2. We was measured at an indenter load of 20 mN.

the diamond indenter during its penetration into the

surface of the film according to Eq. (1). Therefore, this
is also known as plastic hardness. The accuracy of the
hardness measurement, however, decreases for high
hardness values H)60 GPa, because the elastic recovery
We of the film achieves very high values of up to 70
90% and the plastic deformation of the film strongly
decreases (the area between the loading and unloading
curves is very small and represents only 3010% of the
total deformation energy). Therefore, some investigators
suggest use of the universal hardness HU for the
characterization of superhard films. The correctness of
this suggestion also confirms the experiment displayed
in Fig. 6. Here, films with almost the same hardness H

312

J. Musil et al. / Surface and Coatings Technology 154 (2002) 304313

6. Relationships between basic mechanical parameters in hard and superhard coatings

Fig. 14. H 3yE *2 as a function of H for TiSiN, ZrYN, ZrCu

N and TiMoN nanocomposite films sputtered at different deposition conditions, i.e. Ts, Us, is and pN2. H and E * were measured at an
indenter load of 20 mN.

The mechanical behavior of hard and superhard coatings is well characterized, not only by their hardness H,
but also by their effective Youngs modulus E *sEy
(1yn2) and elastic recovery We. Moreover, values of H
and E * measured permit simple calculation of the ratio
H 3 yE *2, which gives information on the resistance of
the material to plastic deformation w8x. The higher this
is, the higher is the ratio H 3 yE *2. The likelihood of
plastic deformation is therefore significantly reduced in
materials with high H and low E *. In general, low E *
is desirable, as it allows the load to be distributed over
a wider area. Typical relationships between H, E *, We
and the ratio H 3 yE *2 for four selected nanocomposite
coatingsTiSiN w11x, ZrYN w12x, ZrCuN w13x
and TiMoN w9xare given in Figs. 1214.
7. Conclusions

exhibit different values of the universal hardness, with

HU being greater for the film with lower penetration of
the diamond indenter into its surface.
The universal hardness HU, however, also exhibits
specific features, and therefore this quantity has to be
used correctly. The main features of HU are the
following.
1. The universal hardness HU first increases with
increasing H, but above some critical value of hardness Hc, HU practically does not change with increasing H)Hc (Fig. 10). This is a direct consequence of
the correction procedure used in the evaluation of the
HU at low values of L.
2. The universal hardness HU depends not only on
hardness H, but also on elastic recovery We of the
film (Fig. 11). HU first increases with increasing
We, but starting at approximately Wef75%, HU
saturates at a value of approximately (i) 20 GPa for
the superhard TiB film and (ii) 11.5 GPa for the
hard AlSiCuN film. This experiment clearly
shows that:
a HU cannot be used to characterize hard films
exhibiting a high elastic recovery WeG80%;
b High values of WeG80% are exhibited not only in
superhard ()40 GPa) films, but also in some hard
(-40 GPa) films; and
c. HU of films with high elastic recovery WeG80%
can have very different values, which are strongly
dependent on their hardness H and effective
Youngs modulus E *.
This experiment shows that the universal hardness HU
cannot be reliably used to characterize superhard films
that exhibit high elastic recovery exceeding 70%.

The main results reported in this paper can be summarized as follows.

1. A comparison of two hard nanocomposite films
shows that the maximum depth dmax of the diamond
indenter impression is higher (i) the lower is H, E *,
H 3 yE *2 and HU and (ii) the higher is the ratio Hy
E * (Tables 1 and 2). This fact does not exclude the
possibility that films with smaller resistance to plastic
deformation (;H 3 yE *2) and lower values of We can
exhibit lower dmax and larger area between the loading
and unloading curves when the ratio HyE * is lower,
compared to films with higher values of H 3 yE *2, i.e.
with (generally) low E * and thus higher HyE * (Fig.
6 and Table 5). This complex relation between the
inherent mechanical properties of hard coatings gives,
however, the possibility of producing films with
different mechanical behavior. This possibility is
based on the fact that a film with a given hardness
H can exhibit substantially different values of E *.
Therefore, very elastic films with high resistance to
plastic deformation (high H 3 yE *2 ratio) or hard films
with high plastic deformation (low H 3 yE *2 ratio) can
be formed (Fig. 6).
2. Hard nanocomposite coatings with very different
hardness can exhibit the same elastic recovery We
(Fig. 5).
3. The same value of the ratio HyE * correlates well
with similar elastic recovery We behavior.
4. The correct value of the hardness of superhard ()60
GPa) films has to be measured at higher loads L,
ranging from approximately 50 to 150 mN, because
only in this interval of L is the hardness
H(L)fconstant. This is a consequence of the fact
that a gradient of the decrease in H with L (increasing
from Ls0) decreases with increasing elastic recovery

J. Musil et al. / Surface and Coatings Technology 154 (2002) 304313

We of superhard films, and the region H(L)fconstant

shifts to higher values of L.
5. The possibility of creating films with similar hardness
and different values of E * allows the tailoring of
films with given mechanical properties.
6. The universal hardness HU cannot be reliably used
for characterization of superhard (G60 GPa) films,
because HU saturates and does not depend on We for
WeG80%.
Acknowledgments
This work was supported in part by the Ministry of
Education of the Czech Republic under Project Nos
MSM 235200002, ME 173y2001 and ME 203y2001.
Constructive comments from the referees of this article,
with regard to presentation of the results, are acknowledged with thanks.
References
w1x E. Broitman, W.T. Zheng, H. Sjostrom,
I. Ivanov, J.E. Greene,
J.-E. Sundgren, Stress development during deposition of CNx
films, Appl. Phys. Lett. 72 (20) (1998) 25322534.

313

w2x L. Karlsson, L. Hultman, J.-E. Sundgren, Influence of residual

stresses on the mechanical properties of TiCxN1yx (xs0, 0.15,
0.45) thin films deposited by arc evaporation, Thin Solid Films
371 (2000) 167177.
w3x A. Matthews, A. Leyland:, Harterei-Tech.
Mitt. 56 (1) (2001)

5.
w4x J. Musil, P. Karvankova,

J. Kasl, Surf. Coat. Technol. 139

(2000) 101.
w5x J. Musil, J. Vlcek,
Surf. Coat. Technol. 142144 (2001) 557.

w6x C. Friedrich, C. Berg, E. Broszeit, C. Berger, Thin Solid Films

290y291 (1996) 216.
w7x N. Kikuchi, M. Kitagawa, A. Sato, E. Kusano, H. Nanto, A.
Kinbara, Surf. Coat. Technol. 126 (2000) 131.
w8x T.Y. Tsui, G.M. Pharr, W.C. Oliver, et al., Mater. Res. Soc.
Symp. Proc. 383 (1995) 447.
w9x F. Regent, J. Musil, Surf. Coat. Technol. 142144 (2001) 146.
w10x S. Veprek, J. Vac. Sci. Technol. A 17 (5) (1999) 2401.
w11x J. Musil, H. Jankovcova,
V. Cibulka, Czech. J. Phys. 49 (3)
(1999) 359.
w12x J. Musil, H. Polakova,

Surf. Coat. Technol. 127 (1) (2000)

99.
w13x J. Musil, P. Zeman, H. Hruby,
P. Mayrhofer, Surf. Coat.
Technol. 120y121 (1999) 179.