Acta mater.

49 (2001) 35393551
www.elsevier.com/locate/actamat

AN ANALYSIS OF LOADPENETRATION CURVES FROM

INSTRUMENTED INDENTATION
K. ZENG and C.-h CHIU
Institute of Materials Research and Engineering, 3 Research Link, Singapore 117602

( Received 6 October 2000; received in revised form 8 June 2001; accepted 8 June 2001 )

AbstractA new empirical method is proposed for analyzing nano-indentation loaddisplacement curves.
This method is based on experimental results and finite element (FEM) calculations reported in the literature.
This method proposes to link the indentationunloading curve to elastic modulus and strain-hardening proper-
ties. Through the analysis, elastic modulus, yielding stress and strain hardening properties are derived from
the complete indentation loaddisplacement curve. This new method has then applied to the nano-indentation
experiments of 14 different materials in which the elastic modulus ranges from 3 to 650 GPa and the hardness
ranges from 0.1 to over 30 GPa. The elastic modulus, hardness and yielding stress derived from the new
method agreed well with the literature values. An analysis of the loading curve also shows that there is a
transition region, in which of the exponent of the loading curve changes from 1.5 to 2 corresponding to the
change of the loads from low to high. This implicates that to avoid this transition region in loading curve,
one should keep the load of the nano-indentation larger than approx. 30 mN. 2001 Acta Materialia Inc.
Published by Elsevier Science Ltd. All rights reserved.

Keywords: Nano-indentation

1. INTRODUCTION simple relationship for the indentation work, the hard-

Instrumented indentation such as nano-indentation
has been a popular technique for measuring the mech-
anical properties of surface of bulk materials and thin
films [112]. The nano-indentation equipment was
first introduced in early 1980s [e.g. 1], providing the
capability to record the loadpenetration curves dur-
ing the loading and the unloading process. It was
recognized by Doerner and Nix that the slope of the
unloading curve at the initial stage of unloading could
be adopted to measure Youngs modulus of the
materials [3]. Their method was later modified by Oli-
ver and Pharr [4, 5] to take into account large elastic
recovery during unloading. The assumptions and limi-
tations inherent in these methods were reviewed in
[6]. More recent development in this direction
focused on new schemes for determining the contact
area at the maximum loading, a crucial quantity for
deriving Youngs modulus. For example, it was pro-
posed in [13] that the contact area could be evaluated
by a polynomial function of the indentation depths at
the maximum unloading and at the end of unloading.
The scheme in [14], on the other hand, was based a
To whom all correspondence should be addressed. Tel.:
+65-874-8495; fax: +65-872-0785.
E-mail address: ky-zeng@imre.org.sg (K. Zeng)
ness, and Youngs modulus.
In contrast to the unloading curves, analyses for the
loading data started much earlier than the introduction
of nano-indentation machine [e.g. 15]. It is now well
recognized that the loading curves of the conical,
Vickers, and Berkovich indenters depend on the
yielding stress, the strain-hardening property, and the
elastic moduli of the materials [79, 15]. Those
results provide fundamentals for employing the sharp
indentation technique to measure the yielding stress
and the strain-hardening parameter. However,
because the shapes of those sharp indenters are self-
similar (ignoring the small imperfection at the
indenter tips), the loading curve can provide only one
independent quantity, which is a combination of the
elastic and the plastic properties of the materials [16].
In order to realize the potential application of sharp
indentation in measuring the yielding stress, it is
necessary to identify another characteristic in the
indentation data that depends on one of the plastic
properties. This issue was addressed in [13], which
proposed that the strain-hardening parameter could be
related to the unloading penetration depth ratio or the
indentation work ratio. The proposed scheme was
shown to be valid by finite element (FEM) calcu-
lations, but it has not been widely tested in experi-
ments. One potential concern of the scheme is that

1359-6454/01/$20.00 2001 Acta Materialia Inc. Published by Elsevier Science Ltd. All rights reserved.
PII: S 1 3 5 9 - 6 4 5 4 ( 0 1 ) 0 0 2 4 5 - 2
3540 ZENG and CHIU: INSTRUMENTED INDENTATION
0.5% error in the measurement of the indentation
work ratio can lead to 20% deviation of the yielding
stress [17].
In this paper, we propose another scheme for using
sharp indentation to derive the elastic and the plastic
properties of materials. The key feature of the scheme
is the proposal that the unloading curve in indentation
can be used to determine both Youngs modulus and
the strain-hardening parameter. This scheme is an
empirical method based on the experimental obser-
vation as well as on the finite element calculations in
[9]. Combining the two properties derived from the
unloading process with the information from the load-
ing curve [8] leads to the yielding stress. In order to
examine the new empirical method, we carried out
nano-indentation experiments of 14 different
materials where the elastic modulus ranges from 3 to
650 GPa and the hardness range from 0.1 to 30 GPa.
The results are shown to be consistent with the litera-
ture values and with those derived from other analysis
methods for indentation data.
The outline of the paper is as follows. Section 2 is
a briefly review of the existing methods for analyzing
the loading curves, the unloading curves, the contact
stiffness, the contact area, the hardness, and the elas-
tic modulus. Section 3 describes the experimental
details and the materials employed in this study of
nano-indentation. Section 4 summarizes the results
based on Oliver and Pharrs analysis scheme for
nano-indentation [4]. Section 5 presents our finding
on the initial part of loading curves. Section 6 intro-
duces the new empirical method for interpreting the
unloading curve. Application of this new method to
determining the yielding stress is discussed in Section
7, followed by discussion and summary in Sections
8 and 9, respectively.
2. REVIEW OF THE EXISTING METHODS
2.1. Loading curve
The loading part of an instrumented indentation
can be expressed as
P Ch2 (1)
where P is the indentation load, h is the penetration
depth measured from surface, and C is a constant
depending on the geometry of the indenter tip and
material properties. The relation in equation (1) has
been demonstrated by numerical simulation for both
elasticperfect plastic and elasticplastic materials
[79, 12, 14, 1621]. The constant C in equation (1)
can be found in [79, 12, 21], based on different
approaches. The results obtained by the finite element
analysis [8] is cited below, which considering a sharp
Berkovich indentation on an elastic material,
E 2
P 2.1891(10.21n0.01n20.41n3) h (2)
1n2
and that on an elasticplastic material,
P
1.273
(tan 24.7)21
su
sy
1 ln
E tan 24.7
3sy
sy h 2
(3)
where n is Poissons ratio, E is Youngs modulus, sy
is the yielding stress, su is the stress at 29% strain,
and the ratio su/sy is used to represent the strain-hard-
ening property of materials throughout this paper. For
convenience, equation (2) is called the indentation
elastic solution, while equation (3) is called the inden-
tation elasticplastic solution of loading.
2.2. Unloading curve and elastic modulus
The unloading curve is generally used to derive the
elastic modulus of the material by the following for-
mula,
E S
(4)
1n2 aA
where S = dP/dh is the contact stiffness at the initial
of unloading process, A is the true contact area at the
maximum load, and a = 1.168 for Berkovich inden-
tation [7, 8], 1.142 for Vickers indentation [7, 8, 22],
and 1.129 for conical indentation [22].
The contact stiffness S can be determined by two
fitting methods for the unloading curves. The first one
is the linear curve fitting method developed by
Doerner and Nix [3], who proposed that Sneddons
flat punch solution [23] could be used to describe the
unloading curve,
P S(hh0) (5)
where h0 is the true contact indentation depth. The
best-fit results of S and h0 depend on the portion of
the unloading curve that is employed in the fitting,
and it is suggested that to use the top one-third of the
unloading data [3].
Equation (5) is based on the assumption that the
contact area remains unchanged during unloading,
which is true for the case of a punch indenting an
elasticperfect plastic material. The solution is there-
fore called the indentation plastic solution in this
paper.
Doerner and Nixs method in equation (5) can
describe well the unloading behavior of most metals,
but often fails to capture that of hard materials such
as ceramics. In order to resolve this issue, Oliver and
Pharr [4, 5] introduced the second method, taking into
account the large elastic recovery during the
unloading process of hard materials. In their scheme,
the power-law relation,
P B(hhmin)m, (6)
 ZENG and CHIU: INSTRUMENTED INDENTATION
is adopted to fit the whole unloading curve where B
and m are the fitting parameters, and hmin is the
remaining plastic indentation depth recorded at the
end of the unloading process. After the parameters B
and m are determined, the contact stiffness can be
evaluated to be S = mB(hmaxhmin)m1 where hmax is
the indentation depth at the maximum load.
One of the major difference between Doerner and
Nixs and Oliver and Pharrs methods is the
approaches for determining the contact stiffness and
how they determine the contact area at the maximum
load, while they both focus on the effects of the elas-
tic modulus on the indentation unloading curves. The
dependence of the curves on the other mechanical
properties was examined in [14, 16, 18], and the
attention was to demonstrate that equation (1) is valid
for a wide range of yielding stress and strain harden-
ing [16, 19]. Those previous studies, however, have
overlooked the shape of the unloading curves and its
relation with the mechanical properties. This issue is
addressed in this paper later in Sections 6 and 7, and
it is shown that the unloading curves can be adopted
to determine Youngs modulus and the strain-harden-
ing parameter.
2.3. True contact area
It is now generally realized that a crucial step in
analyzing the loadpenetration curve of indentation is
to determine the true contact area. For an ideal sharp
Berkovich indenter, the contact area A is given by:
A 24.56h2p (7)
where hp the plastic contact depth at the maximum
load. In Doerner and Nixs method [3], hp is equal to
the fitting parameter h0 in equation (5). In Oliver and
Pharrs method [4, 5], the plastic contact depth hp is
taken to be:
Pmax
hp hmaxe (8)
S mechanical polished using diamond suspensions
where the geometric constant e is taken to be 0.75
for the Berkovich indenter. More recently, Giannako-
poulos and Suresh [13] proposed that the contact area
could be expressed as a polynomial function of the
depth ratio hmax/hmin or the ratio of the total work dur-
ing loading to the elastic work during unloading.
2.4. Hardness
The hardness of a material is defined to be
Pmax
H (9)
A lime glass, Al2O3, and ZrO2), the indentation method
where A is the true contact area at the maximum load.
The area A can be determined by the methods men-
tioned earlier in the previous subsection.
3541
2.5. Elastic modulus of indenter
When indenting a hard material, the indenter defor-
mation can become significant, causing the contact
stiffness to decrease. This effect can be taken into
account by considering the effective contact modulus
Er of the system,
1 1n2 1v20
(10)
Er E E0
where E0 and n0 are Youngs modulus and Poissons
ratio of the indenter, respectively. Equation (10) indi-
cates that the effective contact modulus Er of the sys-
tem is identical to that of the indented material if the
indenter is rigid. The difference between Er and
E/(1n2) increases as the elastic modulus of the
indented material approaches that of the indenter.
Take the diamond indenter as an example. The rela-
tive difference between Er of the system and E/(1
n2) of a material with n = 0.25 will exceed 10% if
Youngs modulus E is larger than 150 GPa.
3. MATERIALS AND EXPERIMENTS
In our study, the following materials are tested by
nano-indentations: soda-lime glass, fused silica, Al,
Cu, Ni, W, Si (001), Stainless steel (301), WC6%
Co, Al2O3, ZrO2, sapphire (random orientation),
glassy carbon, and polycarbonate. Among all these
materials, Al, Cu, Ni, W, glassy carbon, sapphire and
polycarbonate are purchased from Goodfellow Cam-
bridge Ltd (UK). Fused silica is the material provided
by MTS Nano Instruments Innovation Center (USA)
as a standard material for nano-indenter calibration.
Al2O3 is fine-grained polycrystalline ceramics from
Sandvik Procera (Sweden), ZrO2 is 3% Y2O3 partial
stabilized ceramics. Stainless steel is a commercial
steel (301) from our workshop. WC6% Co is a com-
mercial cutting tool insert. All the material was first
(down to 1 m) and then using 0.1 m silica solution
except glass, fused silica, glassy carbon, sapphire and
polycarbonate. The last five materials were tested as
the as-received materials. The literature values of
elastic modulus and yielding stress of these materials
and the sources of the data are listed in Table 1.
The nano-indentation experiments were performed
at two machines, both using Berkovich indenter tips.
Following materials were tested by Nano IIs Nano-
indenter (MTS Cooperation, Nano Instruments Inno-
vation Center, TN): soda-lime glass, fused silica,
Al2O3, ZrO2, and glassy carbon. The load was selec-
ted as 40 and/or 50 mN. For some materials (soda-
suggested by Oliver and Pharr [4] was used, i.e.,
repeated loading and unloading four times at the
maximum load. For those materials, the analysis was
performed on all the four unloading cycles, but the
3542 ZENG and CHIU: INSTRUMENTED INDENTATION

Table 1. Literature values of elastic modulus of the materials 4. EXPERIMENTAL RESULTS

Materials Elastic modulus (GPa) Yielding stress (GPa)
Table 2 summarizes the hardness H and Youngs
Fused silica 6973 a

modulus E derived from Oliver and Pharrs power
Glassy carbon 2030b law fitting method, including the average value and
Soda-lime glass 66a the standard deviation of the two properties. Compar-
ZrO2 (PSZ) 205a
Al2O3 380a ing the results with Table 1 indicates that the elastic
Polycarbonate 2.5b 0.07g modulus measured by indentation is generally higher
Al 68.3c 0.10.2b than those reported in the literature.
Cu 117132b 0.070.4f
Si 112c Different maximum loads were also adopted in our
Sapphire 440.0d experiments. For the length of the paper, however,
Ni 207.0c 0.5h
Stainless steel 301 175215e 1.11.9e
the results will be presented elsewhere.
W 400.0f 0.551.0h
WC6% Co 614650f 6.0f,i
5. ANALYSIS OF LOADING CURVES
a
Engineered Materials Handbook, Volume 4, Ceramics and Glasses,
ASM International, 1991. All the numerical analyses for cone, Vickers, and
b
The Materials Selector, Vols. 2 and 3, 2nd edn, ed. N. A. Waterman Berkovich indentations indicated that the loading
and M. F. Ashby, Chapmam & Hall, London, 1997.
c
Matallic Materials Specification Handbook, 4th edn, ed. R. B. Ross, curve follows equation (1) [79, 22, 23]. Many
Chapman & Hall, London, 1992.
d
experimental results, however, have shown that the
Oliver, W. C. and Pharr, G. M., J. Mater. Res., 1992, 7(6), 1564.
e
ASM Special Handbook, Stainless Steels, ASM International, 1994.
actual relation between the load P and penetration
f
ASM Metals Handbook, Vol. 2, Properties and Selection, ASM Inter- depth h deviates from the theoretical prediction. For
national, 1992. example, when fitting the loading curve to a power-
g
CRC Materials Science and Engineering Handbook, 2nd edn. CRC
Press, 1994. law relation, P = Chn, the derived exponent n is less
h
Materials Data Sheet. Goodfellow Cambridge Ltd, 1999. than 2 [24, 25]. The discrepancy between the experi-
i
Compressive strength. mental and the theoretical results poses an issue on
understanding the loading curves obtained in experi-
ments, as well as the material properties derived by
result presented in the paper is only from the last interpretation of the curves. Therefore, it is necessary
unloading cycle. For the rest of materials, the tests to have an insight into the discrepancy before adopt-
were performed using UMIS-2000H Nano-indenter ing any model for the indentation loading curves.
(CSIRO, Australia). Again, the load was selected as The following comparison scheme is adopted to
40 and/or 50 mN. Due to the set-up of the UMIS- have a better picture about the discrepancy between
2000 Nano-indenter, Oliver and Pharrs experimental the experimental and theoretical results. In the
method cannot be used, therefore all the tests on this scheme, the loading curve is contrasted with the two
machine (UMIS-2000H) were only have one loading lines, P = C1h3/2 and P = b + C2h2, corresponding to
and unloading cycle. the cases of spherical and sharp Berkovich inden-
The indentation procedure used as following: load- tation, respectively. The constant C1 is determined by
ing to the maximum load in 20 s, holding for 30 s at fitting the first function to the initial part of the load-
the maximum load, and then unloading in approxi- ing curve (first 2050 data point). And the constants
mately the same rate (20 s from the maximum load b and C2 corresponds to the best fit of the second
to 90% of the unloading). At the 90% of unloading, function to the last part of the loading curve (last 30
another holding of 20 s to correct the thermal draft, 50 data point from the maximum load).
then fully unloading to the zero-load. This procedure The comparison scheme is applied to the cases of
was used at both Nano IIs and UMIS-2000H nano- fused silica, aluminum, and ZrO2, and the results are
indenters. The experimental data were analyzed using depicted in Fig. 1(ac), respectively. The figure
the power-law method [4] to derive the elastic modu- shows that the loading curves for those materials are
lus equations (6)(10). At least 10 indents were per- described by two different functions, P = C1h3/2 and
formed at the selected load. The reason to select the P = b + C2h2, at low- and high-loads, respectively.
indentation loads of 40 and/or 50 mN is discussed in The transition of the characteristics of the loading
Section 5. curve suggests it is the initial indentation that causes
It is worth to note that our experimental work the exponent n in the fitting P = Chn to deviate from
covers 14 materials range from polymer, soft and hard 2. The initial deviation may come from the initial
metals, ceramics, to hard carbide materials. The elas- contact at the surface and/or the imperfectness of
tic modulus and hardness of these materials covers a indenter tip. These effects become insignificant as the
range with 23 order of magnitude of differences. The load increase. Therefore, the loading process in
work was done over two different nano-indentation experiments will follow closely the theoretical predic-
machines. In addition, several indenter tips were used tion given in equation (1) after the load is sufficiently
during the experiments. Therefore the analysis and large. The minimum load required for equation (1) to
the results presented in this paper should have very be valid varies with the hardness of the material as
wide representative and unique future. well as the shape of the indenter tip. As a rule of
 ZENG and CHIU: INSTRUMENTED INDENTATION 3543

Table 2. Summary of results from the power-law fitting analysis

Materials Load (mN) E (GPa) H (GPa) Instrument

Fused silica 50 79.50.3 10.80.05 Nano IIs

Glassy carbon 50 12.60.8 1.90.3 Nano IIs
SLS-glass 35 95.710.7 6.40.6 Nano IIs
SLS-glass 50 80.20.5 7.10.06 Nano IIs
Nano IIs, four times
SLS-glass 40 80.10.2 7.60.07
unloading
Nano IIs, four times
ZrO2 40 310.611.2 20.21.2
unloading
Nano IIs, four times
Al2O3 40 474.441.3 34.84.0
unloading
Polycarbonate 40 3.20.05 0.180.01 UMIS-2000H
Al 40 97.89.0 0.70.05 UMIS-2000H
Al 50 66.616.0 0.70.2 UMIS-2000H
Cu 40 122.817.0 1.50.1 UMIS-2000H
Si (001) 40 175.014.3 13.01.5 UMIS-2000H
Sapphire 40 418.84.8 29.30.8 UMIS-2000H
Ni 40 204.26.2 2.70.2 UMIS-2000H
Stainless steel 40 206.19.6 3.70.1 UMIS-2000H
W 40 431.89.1 10.80.4 UMIS-2000H
WC6% Co 40 578.318.9 24.41.5 UMIS-2000H

thumb, the load should be larger than 30 mN in order
for nano-indentation to be beyond the transition
region. For this reason, the indentation loads have
been selected to be 40 and/or 50 mN in our experi-
ments.
The requirement of a minimal load has an
important implication on the indentation of
film/substrate structures. In general, the indentation
loading curves of film/substrate systems will deviate
from equation (1) at high loads because of the sub-
strate effect. On the other hand, the minimal require-
ment suggests the loads have to be sufficiently large
in order to avoid the complications at the initial stage
of loading. The restrictions at low and high loads
become an issue when the film thickness is too small
such that even the minimal load can cause significant
substrate effect. As a simple estimation, this situation
can occurs when the film thickness is less than 10
times the indentation depth at the minimal load of
30 mN. It follows from the results in Fig. 1 that the
corresponding film thickness is about 3, 5, and 20 m
for ZrO2, fused silica, and Al, respectively. However,
a typical Al film on Si is usually less than 1 m in
thickness. Obviously, how to analyze the loading
curves in those cases is still an open question.
6. AN EMPIRICAL METHOD FOR ANALYZING
UNLOADING CURVES
In this section, an empirical method for analyzing
the unloading curves of sharp Berkovich indentation
is first proposed, taking into account the effects of
elastic modulus and strain hardening on the unloading
curves. This empirical method is then adopted to ana-
lyze our experimental data, which demonstrates that
the new method fits well the unloading curves
recorded in the experiments when the load is suf-
ficient high. Application of the method to deriving the
mechanical properties of materials, including
Youngs modulus E, the strain-hardening parameter
su/sy, and the yielding stress sy, is presented in the
next section.
General speaking, the characteristics of the inden-
tationunloading curves and their dependence on the
stressstrain properties of a general elasticplastic
material are not fully understood. However, a trend
of the indentationunloading curves can be uncovered
when examining the results of two extreme cases
where the materials are fully elastic and elastic per-
fectplastic, respectively. For a fully elastic material,
the indentationunloading curve will be identical to
the loading one as described in equation (2), i.e. a
parabolic curve Ph2. The indentationunloading
curve of an elastic perfectplastic material, on the
other hand, can be approximately described as a
straight line depicted in equation (5) if the yielding
strain is not unreasonably large, say 10%. For the
general elasticplastic material, the stressstrain
relation is between elastic one and elastic perfect
plastic one. Thus, the indentationunloading curve of
the general elasticplastic material will also be
between a parabolic curve and a straight line; as sche-
matically illustrated in Fig. 2. The experimental data
presented in Fig. 3 shown clearly that the unloading
curve is bounded by two lines (corresponding to the
indentation of fully elastic and elastic perfectplastic
cases), this also confirmed by the FEM calculations
presented in [9]. The unloading curve will be close
to a straight line if the material is an almost elastic
perfectplastic one, i.e., if the strain hardening para-
meter is small. In contrast, the unloading curve will
be close to a parabolic curve if the strain hardening
parameter is large. This suggests the unloading curve
could be written as a linear combination of the results
of the two extreme cases as below:
P (1q)f(n)Eh2 qS(hh0) (11)
where (1q) and q, respectively, are the weight of
3544 ZENG and CHIU: INSTRUMENTED INDENTATION
Fig. 1. Indentation loading curves of (a) fused silica, (b) Al
and (c) ZrO2 at different loads.
the elastic and the elasticperfect plastic responses in
the unloading curve, f(n) is the effect of Poissons
ratio n on an elastic indentation, S is the unloading
stiffness of indentation on an elasticperfect plastic
material, and h0 is a constant, referring to the plastic
depth of an indentation on the elasticperfect plastic
material. It follows from equations (2), (4) and (7)
that f(n) and S for Berkovich indentation are given by,
2.1891(10.21n0.01n20.41n3)
f(n) , (12)
1n2
Fig. 2. Schematic representation of relation of the stressstrain
characteristics to the indentation loaddisplacement curve (a)
elastic, (b) elasticplastic, (c) elasticperfect plastic and (d)
rigid plastic.
Fig. 3. Experimental data showing the indentationunloading
curve is bounded by elastic solution and plastic solution.
24.56 E
S2 h. (13)
p 1n2 0
Substituting equations (12) and (13) into (11) leads to
24.56 E
P (1q)f(n)Eh2 2q h (hh0).
p 1n2 0
(14)
Equation (14) is an empirical equation for analyzing
the unloading curve of Berkovich indentation on a
general elasticplastic material.
The weight q mainly depends on the strain harden-
ing parameter sy/su. When sy/su = 1, corresponding
to an elasticperfect plastic case, q = 1. On the other
hand, when sy/su = 0, corresponding to an elastic
case, q = 0. According to the two results, it seems
reasonable to assume the following relation for strain-
hardening and unloading curve,
q sy/su. (15)
There clearly exist other empirical expressions for q
that satisfy the two results at sy/su = 0 and 1. One
 ZENG and CHIU: INSTRUMENTED INDENTATION
example is a power-law expression such as
q = (sy/su)m. Which expression is better for describ-
ing the dependence of q on the strain-hardening para-
meter requires further theoretical analyses for the
unloading process. This is a challenging question, and
is still under investigation in our group. In spite of the
lack of a rigorous theoretical support, the empirical
expressions in equations (14) and (15) together with
the loading relation equation (3) seem to provide
good estimations for the yielding stresses. As shown
later in Section 6, the yielding stresses derived by
adopting these three equations are consistent with the
literature values obtained by other experimental tech-
niques.
Another question concerning the expression for q
is its dependence on the yielding strain sy/E. This
issue is addressed later when we discuss Table 5,
which shows little correlation between q and sy/E for
the materials tested in our experiments.
Now turn to the data analysis process for fitting
equation (14) to experimental results. It may be first
noted that equation (14) is a second order polynomial
of h with three unknown parameters q, E, and h0,
assuming n is known. This seems to suggest that one
can first fit the second order polynomial equation
P = ah2 + bh + c to the experimental data, determine
the coefficients a, b, and c, and then use the coef-
ficients and equation (14) to evaluate q, E, and h0.
This approach, however, will lead to wrong results
since the fitting does not take into account the limits
on the values of q, E, and h0 in the actual situation.
The finding led us to adopt Bates and Watts
method for bounded fitting parameters [26] together
with the chi-square fitting scheme [27] when analyz-
ing our experimental data. The details of Bates and
Watts method and the implementation for the current
study are presented in Appendix A. Here it is suf-
ficient to explain the range of the value of each para-
meter,
1q0, E0, hhmaxh0hmin (16)
where hmax and hmin are the recorded maximum and
minimum penetration depth during unloading, and the
parameter h, depending on the materials, is taken to
be 1 or 1.1. The first option h = 1 is adopted for hard
materials such as fused silica, glass, ZrO2, Al2O3,
WCCo, and sapphire. And the second option
h = 1.1 is employed for metallurgical materials such
as Al and Cu.
Choosing a higher value of h reflects the fact that
there is pile-up around indents in the cases of inden-
tation on metallurgical materials such as Al, Cu, Ni,
and stainless steel. The pile-up causes the effective
penetration depth in those materials to be larger than
the depth recorded in the experiments; see Fig. 4.
Accordingly, the parameter h0, which is related to the
plastic penetration depth, should be allowed to exceed
the recorded maximum depth hmax, or equivalently h
3545
Fig. 4. Schematic drawing showing the surface displacement
during the indentation and the relations between h0 and hmax,
(a) no pile-up or sinking-in, (b) sinking-in, and (c) pile-up.
has to be larger than 1. A question raised is how to
choose the value h. Our calculation suggests if is
sufficiently large, the actual choice of h has little
effect on the final fitting result since h only deter-
mines the upper bound for the fitting parameter h0.
When h is too large, however, the iteration needed to
obtain a convergent fitting result will increase drasti-
cally. This suggests that the optimum value of may
be the extent of pile-up. Assuming the maximum pile-
up is about 10% of hmax leads to the choice h = 1.1
for Al and Cu in the current study.
The chi-square fitting in the current study is non-
linear since the empirical equation, given in equation
(14), depends non-linearly on the fitting parameters
q, E, and h0. The fitting thus requires iterations in
order to obtain the best-fit parameters that minimize
a c2 merit function. The iteration scheme in our calcu-
lation was adopted to be the LevenbergMarquardt
method [27]. And the initial values of q, E, and h0
for the iterations were chosen as follows: q = 0.5,
E = 100 GPa, and h0 = (hhmax + hmin)/2. The only
exception was the initial value of q for Al and Cu,
which was taken to be 0.88 in order to accelerate the
convergence of the iteration results.
Our data analyses for the unloading curves focused
on fitting equation (14) to the first part of curves
where P was generally higher than approx. 20 mN.
In other words, only the top 50% of the unloading
curves recorded in our experiments were adopted in
the fitting process. In this range of loading, the
empirical expression in (14) fits well the unloading
curves. The best-fit parameters in the expression
remained insensitive even when a smaller part of the
curves were employed in the data analyses. The best-
fit parameters, however, could change significantly if
some of the last part of the unloading curves was
included in the analyses. The last part of the
unloading curves when unloading to below approx.
20 mN cannot be well described by our empirical
expression in (14).
3546 ZENG and CHIU: INSTRUMENTED INDENTATION
The failure of equation (14) in capturing the last
part of the unloading curves can be explained by our
earlier finding in Fig. 1 that the loading curves deviate
from the theoretical prediction for a sharp indentation
in the range of 2030 mN during loading. We have
found that there is a transition region at the load
approx. 2030 mN during loading. The finding sug-
gests the unloading curves will also deviate from the
prediction based on the sharp indentation assumption,
our fitting results showed that this deviation occurs
when the load P is below approx. 20 mN in our
experiments. Since the assumption is indeed implied
in equation (14), the equation is therefore inappropri-
ate for the last part of the unloading curve. This
explanation was verified by carrying out Berkovich
indentation tests on a few materials, such as ZrO2,
with higher loads of 75 and 100 mN. It was found
that the unloading curves in these tests could be well
described by equation (14) in the same part of curves
where P is higher than approx. 20 mN.
Parts (ah) of Fig. 5 compare the unloading data
in the experiments with the fitting results of fused
silica, Si, Cu, ZrO2, polycarbonate, sapphire, stainless
steel 301, and tungsten, respectively. The results dem-
onstrate that equation (14) fits well the high load part
of the unloading curves in our experiments. The
empirical equation can even capture almost the whole
unloading curves in the cases of fused silica, Cu,
sapphire, stainless steel 301, and tungsten although
only about 50% of data were used in our fitting.
7. ELASTIC MODULUS, STRAIN HARDENING,
YIELDING STRESS, AND PILE-UP
This empirical method for analyzing loading and
the unloading curves of Berkovich indentation,
expressed in equations (3), (14), and (15), provide a
new data analysis scheme for determining Youngs
modulus E, the strain-hardening parameter su/sy, the
yielding stress sy, and the occurrence of pile-up or
sinking-in by the indentation technique. The first step
of the scheme is to fit equation (14) to the indentation
unloading curves subject to the constraints given in
equation (16). Combining the results with the
assumption in equation (15) yields Youngs modulus
E, the strain-hardening parameter su/sy, and h0 of the
materials; the ratio h0/hmax indicates the occurrence of
pile-up (h0/hmax1) or sinking-in (h0/hmax1). The
second step is to fit the function P = Ch2 to the load-
ing curves. Substituting the coefficient C and the
results of E and su/sy derived in the first step into
equation (3) determines the yielding stress sy.
The quantity h0 is the only fitting parameter that
has a dimension of length in our method. We can
therefore define the hardness of the material as
P between the strain hardening exponent determined
H (17)
24.56h20
The hardness is called the perfect plastic hardness
(PPH) since h0 is the effective plastic depth of the
elasticperfect plastic contribution during indentation.
The analysis scheme was applied to the indentation
data of the materials tested in our experiments. The
results of E, sy, su/sy, h0, and the PPH hardness are
summarized in Table 3. The results demonstrate that
Youngs modulus E derived by the new analysis
scheme compares well with the literature values listed
in Table 1 and with those in Table 2 that were evalu-
ated by using Oliver and Pharrs scheme [4] to fit our
experimental data. The derived yielding stresses sy in
most of the cases also agree well with the literature
values. In only two cases, Cu and W, the results are
only slightly higher than the literature values. The
reasonable agreement between our results and the
literature values suggests that the empirical
expressions, equations (14) and (15), can be used to
describe well the unloading process.
Throughout this paper, the strain-hardening para-
meter of a material is represented by the ratio su/sy
as suggested by FEM numerical calculations [8]. The
parameter can be used to determine the other strain-
hardening properties defined in some well-known
material models for plastic deformation. One example
is the power-law model where the stressstrain
relation under uni-axial tension in the range of yield-
ing can be described as
s sy
e n
ey
. (18)
In equation (18), ey = y/E is the yielding strain, and
n is the strain-hardening exponent. The exponent n is
related to su/sy and ey by
ln(su/sy)
n (19)
ln(eu/ey)
Using eu = 0.30 and ey = 0.002 leads to equation (1)
in [17], while in our calculation, eu was taken to be
0.29 [79] sy was not fixed at 0.002 but evaluated
by sy/E. The calculated results of the strain-hardening
exponent n of the materials tested in our experiments
are presented in Table 4 where the values of E, sy,
and su/sy given in Table 3 are employed in the calcu-
lation. The results indicate that the magnitude of the
exponent n is in the range from 0.01 to 0.03 for the
metals tested in our experiments, while n is larger
than 0.2 for the polymers, the glass, the carbide, and
the ceramics examined here. It is known that most of
metallic materials can exhibit a wide range of strain
hardening exponents (0.0n0.6) depending on the
composition and treatment conditions (annealed or
work hardened etc.) [17]; therefore a comparison
from equation (19) with literature values need to be
studied further.
 ZENG and CHIU: INSTRUMENTED INDENTATION 3547

Fig. 5. Curve fitting of the indentation unloading curve by equation (14) of selected materials: (a) fused silica,
(b) Si (001), (c) Cu, (d) ZrO2, (e) polycarbonate, (f) sapphire, (g) stainless steel 301, and (h) tungsten.

Equations (18) and (19) suggest a method for using
the sharp indentation technique to construct the
stressstrain relation; however, the method is only
valid when the power-law model for plastic defor-
mation is appropriate for the material. The sharp
indentation technique does not have the capability to
depict the detailed stressstrain relation as provided
by a tensile test since a sharp indentation test can only
apply a characteristic strain on the system, irrespec-
tive of the indentation loading [7, 13, 15].
The actual physical meaning of the parameter h0 in
our empirical method has not been fully understood,
while it is noted that the ratio h0/hmax seems to be
correlated with the occurrence of pile-up or sinking-
in during indentation. For example, the ratio h0/hmax
of metallurgical materials, especially Al and Cu, is
larger than unity in our fitting, and a significant pile-
up is usually observed in these materials during
indentation. For some hard metals such as Ni, stain-
less steel, and W, h0/hmax is close to unity and the
 3548

Table 3. Summary of results from the new analysis

Material Load (mN) E (GPa) q h0 (nm) PPH (GPa) Yielding strength (GPa) Instrument

Fused silica 50 74.01.1 0.490.04 430.612.1 11.00.6 2.560.22 Nano IIs

Glassy carbon 50 10.30.6 0.080.01 1474.743.1 0.950.06 0.0650.006 Nano IIs
SLS-glass 35 81.26.0 0.530.04 507.125.1 5.580.53 2.210.16 Nano IIs
SLS-glass 50 79.52.5 0.460.02 644.619.6 4.910.32 1.900.10 Nano IIs
Nano IIs, four
SLS-glass 40 74.41.1 0.430.04 533.316.9 5.740.36 1.910.20
times unloading
Nano IIs, four
ZrO2 40 275.010.2 0.420.02 337.98.6 14.30.7 4.360.13
times unloading
Nano IIs, four
Al2O3 40 416.632.4 0.310.04 269.513.2 22.62.1 6.510.86
times unloading
Polycarbonate 40 2.140.06 0.490.04 3279.355.6 0.150.01 0.0540.004 UMIS-2000H
Al 40 61.82.8 0.920.04 1576.867.4 0.660.06 0.250.04 UMIS-2000H
Al 50 61.42.8 0.870.004 1794.872.9 0.640.05 0.230.03 UMIS-2000H
Cu 40 99.16.2 0.920.02 1116.229.1 1.310.07 0.600.04 UMIS-2000H
Si (001) 40 132.88.8 0.460.10 415.724.9 9.521.21 2.940.57 UMIS-2000H
Sapphire 40 484.913.4 0.180.05 244.817.9 27.64.62 3.470.99 UMIS-2000H
Ni 40 213.414.0 0.940.01 769.918.6 2.750.14 0.550.04 UMIS-2000H
Stainless steel 301 40 191.46.3 0.930.01 643.515.2 3.940.19 1.140.05 UMIS-2000H
W 40 401.027.5 0.900.03 378.317.0 11.451.20 1.500.54 UMIS-2000H
ZENG and CHIU: INSTRUMENTED INDENTATION

WC6% Co 40 619.522.8 0.430.10 232.712.3 30.313.13 5.771.02 UMIS-2000H

 ZENG and CHIU: INSTRUMENTED INDENTATION 3549

Table 4. Summary of H/E, sy/E, su/sy and strain-hardening exponent n based on new model

Materials H/E sy/E su/sy n

Fused silica 0.149 0.035 2.04 0.337

Glassy carbon 0.092 0.006 12.5 0.651
SLS-glass 0.069 0.026 2.11 0.310
ZrO2 0.052 0.016 2.38 0.299
Al2O3 0.054 0.015 3.23 0.396
Polycarbonate 0.070 0.025 2.05 0.293
Al 0.011 0.004 1.12 0.027
Cu 0.013 0.006 1.09 0.022
Si (001) 0.072 0.022 2.17 0.300
Sapphire 0.057 0.007 5.56 0.461
Ni 0.013 0.003 1.06 0.013
Stainless steel 301 0.021 0.006 1.08 0.020
W 0.029 0.004 1.11 0.024
WC6% Co 0.049 0.009 2.33 0.244

Table 5. Comparison of q and sy/E for some selected materials
Materials q sy/E
Polycarbonate 0.49 0.028
Al 0.92 0.0029
Cu 0.92 0.0034
Ni 0.94 0.0024
Stainless steel 301 0.93 0.0077
W 0.9 0.0025
WC6% Co 0.43 0.0092
experimental observations are consistent that there is
no significant pile-up or sinking-in in those materials.
For the other materials tested here, the ratio h0/hmax
is less than unity, which again is in accordance with
our experimental observations that the sinking-in
occurred during indentations in those materials.
It is emphasized that the data analysis scheme
presented here not only provides a novel recipe for
determining the mechanical properties of materials by
sharp indentation, but also has the advantage of being
robust. The method is applicable to a wide range of
materials including ceramics, hard and soft metals,
polymers and carbide materials. The method yields
consistent results though our experiments involved
two different nano-indentation machines and several
different indenter tips. The method also has the
advantage that it does not require knowledge of true
contact area or tip profile; as a consequence, detailed
calibration of the indenter shape can be avoided in
our analysis.
The fitting parameter q in equation (14) is proposed
to be equal to the strain-hardening parameter sy/su in
this paper. A question raised is whether q is also
related by the yielding strain ey = sy/E. This question
is examined in Table 5 by comparing q with sy/E.
The values of are taken from the fitting results in
Table 3, while those of sy/E are from the literature
results in Table 1. The comparison indicates that the
correlation between q and sy/E is not significant (the
correlation coefficient is 0.72 [28]), and in many
cases q is insensitive to the variation of sy/E. For
example, sy/E of Ni and stainless steel 301 is signifi-
cantly different (0.0024 and 0.0077, respectively), but
the corresponding difference in q is negligible (0.94
and 0.93). Similar situation can also be found in the
comparison of polycarbonate and WC with 6% Co.
These finds seem suggest that the values of q and
sy/E do not have relationship.
8. DISCUSSION
This paper points out a new empirical method for
determining the elastic modulus, strain-hardening
parameter, and yielding stress by sharp indentation.
Supported by the good agreement between the results
and the literature values as well as the finite element
calculation derived earlier [9], the new method has
many potential applications on measuring the mech-
anical properties of complicate structures at small
length scales. The development of the approach,
nevertheless, is still at the early stage, and many
important issues need to be resolved in order to make
significant process in the future.
One of the issues is to explain the empirical method
expressed in equations (14) and (15) from a theoreti-
cal point of view. This method is proposed by using
a simple argument based on the experimental obser-
vations and finite element calculations. Although the
method seems to fit well the experimental data, it is
still necessary to employ the theoretical background
to understand why the unloading curve can be
approximately described by the function given in equ-
ation (14). The understanding will shed a light on the
physical meanings of the two fitting parameters, q and
h0, in the empirical formular and on how the two
parameters are related to the mechanical properties of
the materials. Particularly, it is important to under-
stand the dependence of q on su/sy. It is also neces-
sary to examine the relation between q and the yield-
ing strain ey = sy/E and that between the ratio
h0/hmax and the amount of pile-up/sinking-in during
indentation.
Another issue that needs to be explored is the
indentation unloading process of thin film/substrate
systems. Similar to the case of bulk materials, the
shape of the unloading curves in the systems has been
overlooked in the literature, though the dependence
of the contact stiffness at the initial of unloading on
3550 ZENG and CHIU: INSTRUMENTED INDENTATION
the elastic moduli of the film and the substrate was
examined in [29]. Modifying the results by consider-
ing the effect of strain-hardening on the unloading
process may provide an insight into the unloading
curves of the systems.
The third issue is the uniqueness of the mechanical
properties determined by the sharp indentation test.
This issue was addressed in [30] where FEM calcu-
lations was employed to show that different combi-
nations of yielding stress sy and strain-hardening
exponent n could lead to the same loading and
unloading curves. A more recent study, however,
repeated some of the calculations and concluded that
the loading/unloading curves were different [17]. In
order to clarify this issue, it is necessary to carry out
systematic calculations to examine the variations of
the characteristics of the loading/unloading curves
with the mechanical properties.
The fourth issue is the initial indentation due to
imperfect indenter tip and contact surface. Of parti-
cular interest is how the imperfect indenter tip and
contact surface cause the loading curves to deviate
from the relation P = Ch2 at the initial stage of inden-
tation. An insight into the scenario is an essential part
in developing models for the loading process of thin
film/substrate systems.
9. SUMMARY
This paper focused on the data analysis scheme for
the unloading and the loading curves of nano-inden-
tation experiments and on the mechanical properties
that can be derived from the indentation
load/unloading curves. The model for the loading
curve is adopted to be that expressed in equation (1).
Comparing the model with our experimental results
of loading curves shows that the initial portion of the
loading curve deviates from the theoretical prediction
in equation (1), but the curve approaches equation (1)
as the load increases. The finding enables us to deter-
mine the minimum loads needed in order to adopt
equation (1) to analyze the loading data in the nano-
indentation experiments. It is suggested that the load
should be higher than at least 30 mN for nano-inden-
tation of bulk materials.
A new empirical method for analyzing the
unloading curves in indentation is proposed in equa-
tions (14) and (15). A key feature of the method is
that the unloading curves can be used to determine
the elastic modulus and the strain-hardening para-
meter of the material, and to examine the occurrence
of pile-up or sinking-in during indentation. The
knowledge of the two mechanical properties is parti-
cularly useful since combining the knowledge with
the fitting result of the loading curve leads to another
crucial material property, namely the yielding stress.
This new method makes the nano-indentation tech-
nique a self-sufficient method for determining the
mechanical properties of materials.
Numbers of materials including ceramics, hard and
soft metals, carbide and polymers were tested and
analysed by the new method. The results of Youngs
modulus and the yielding stress of the materials agree
well with the existing literature values. The Youngs
modulus is also consistent with those derived by other
analysis methods for nano-indentation data. The new
method has the advantage of robust, giving consistent
results even though our experiment involved different
nano-indentation machines and indenter tips. The
method also has the advantage that it does not require
knowledge of true contact area or tip profile.
Finally, we defined a new hardness of materials,
called the perfect plastic hardness. The new hardness
related only with the virtual perfect plastic defor-
mation during indentation.
AcknowledgementsPart of the experimental work was done
at Department of Materials Science and Engineering, Royal
Institute of Technology (KTH), Stockholm, Sweden. The
authors would like to thank the support for the experiments
from KTH.
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APPENDIX A
Curve fitting with the bounded fitting parameters and
initial values determination
For a fitting parameter a bounded with fixed values
a and b, it is then more convenient to write the fitting
parameter as:
ba
aa (A1)
1 ef
where as f is a new parameter can take any value
between and +. Based on equation (A1), we
choose the fitting parameters q and h0 as follows
1 by 1.1hmax, this allows maximum pile-up 10% of hmax,
q (A2)
1 ef1
3551
and
hmaxhmin
h0 hmin (A3)
1 ef2
where the new parameters f1 and f2 can have any
value between and +, but the values q and h0
are bounded within their limits.
For the work presented in this paper, two kinds of
initial values were given. For hard materials such as
fused silica, glass, ZrO2, Al2O3, WCCo, sapphire
etc, the initial values were taken as that f1 = f2 = 0.
This gives the q = 0.5 and h0 = 1/2(hmax + hmin).
For soft metallurgical materials, such as Al, Cu, Ni
and stainless steel etc, the initial value was selected
differently. The indentation unloading curve of these
material is close to a straight line, this means that
fitting parameter q is very close to 1. In order to min-
imize the computation time for the non-linear curve
fitting, we choose f1 = 2, gives the initial value of
q = 0.88. For those materials, we also include the
pile-up during the indentation, then set f2 = 0, but the
upper bound for h0 in equation (A3), hmax is replaced
so that the initial value is h0 = 12(1.1hmax + hmin).