Surface & Coatings Technology 200 (2006) 4153 – 4165

www.elsevier.com/locate/surfcoat

Review

Critical review of analysis and interpretation of nanoindentation test data

A.C. Fischer-Cripps*
CSIRO Industrial Physics, PO Box 218, Lindfield NSW 2070, Australia

Received 5 January 2005; accepted in revised form 18 March 2005

Available online 30 April 2005

Abstract

This paper reviews commonly used methods of analysing and interpreting nanoindentation test data, with a particular emphasis on the
testing of thin films. The popularity of nanoindentation testing is evidenced by the large number of papers that report such measurements in
recent years. Unfortunately, there appear to be several issues that are emerging as common sources of error in using this technique. The
present paper is aimed at highlighting these errors for the benefit of those practitioners who wish to use the technique but are not fully
conversant with the field.
D 2005 Elsevier B.V. All rights reserved.

Keyword: Nano-indentation

Contents

1. Introduction . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 4153
2. Indenter . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 4154
3. Contact mechanics . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 4155
3.1. Loading . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 4155
3.2. Maximum load. . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 4156
3.3. Unloading . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 4156
4. Fitting the load – displacement curve . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 4158
5. Corrections . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 4159
5.1. Initial penetration or zero point determination . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 4159
5.2. Frame compliance . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 4159
5.3. Area function . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 4161
5.4. Materials issues . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 4161
6. Interpretation of the results . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 4162
6.1. Elastic modulus . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 4162
6.2. Hardness . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 4163
7. Conclusion . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 4164
Acknowledgement . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 4165
References . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 4165

1. Introduction

Nanoindentation testing is a fairly mature technique

* Tel.: +61 2 9413 7544; fax: +61 2 9413 7547. which uses the recorded depth of penetration of an
E-mail address: Tony.Cripps@csiro.au. indenter into the specimen along with the measured
0257-8972/$ - see front matter D 2005 Elsevier B.V. All rights reserved.
doi:10.1016/j.surfcoat.2005.03.018
4154 A.C. Fischer-Cripps / Surface & Coatings Technology 200 (2006) 4153 – 4165
applied load to determine the area of contact and hence
the hardness of the test specimen. Many other mechanical
properties can also be obtained from the experimental
load –displacement curve, the most straight-forward being
the elastic modulus. Other properties such as the strain-
hardening index, fracture toughness, yield strength and
residual stress can also be obtained in some circum-
stances. The method relies on there being an accurate
determination of the initial contact of the indenter with
the specimen surface, corrections for any penetration that
arises during this initial contact, corrections for compli-
ance of the loading column, corrections for the departure
of ideal shape of the indenter, and corrections for
materials-related issues such as piling-up and indentation
size-effect, residual stress, etc. Review articles and books
provide a good starting point for those entering the field
[1 –5]. However, it is the present author’s experience that
there is emerging a common set of misconceptions and
errors in the application of the technique. The present
paper seeks to highlight these issues for the benefit of
those who are not conversant with the method but wish to
report their work using the best available practices.
2. Indenter
The three-sided Berkovich indenter is the most popular
geometry for nanoindentation testing. A typical Berkovich
indenter tip is shown in Fig. 1. The face half-angle of a
Berkovich indenter used for nanoindentation work is
65.27- å 65.3-. This gives the same projected area to
depth ratio as the more commonly used four-sided Vickers
indenter (face angle 68-) used in microhardness testing. It
is important to distinguish between the projected area of
impression and the actual area of impression. The
projected area is that which is observed when looking
face-on to a residual impression in a specimen surface at
normal incidence to the surface without regard to the
actual sloping sides of the impression. The actual contact
(a)
Fig. 1. (a) High-magnification SEM scan of the tip of a Berkovich diamond indenter and (b) schematic of indenter geometry. A is the projected contact area, h
is the face angle, and h c is the depth of the circle of contact measured from the apex of the indenter.
area is that which does take into account the sloped sides
of the impression. Initially, one might expect that it would
be more correct to always work with the actual surface
area of the residual impression and this is indeed what the
standard Vickers hardness number is based upon. How-
ever, the indentation load, divided by this actual area does
not have a real physical significance other than it has
been found to provide a useful measure of hardness in an
engineering context. When one divides the indenter load
by the projected area of the impression, one obtains the
mean contact pressure which is a physical quantity. The
connection between the hardness of a material and the
mean contact pressure has some particular importance,
especially for thin film specimens and this will be
discussed in a later section.
Experience shows that the face angles of a Berkovich
indenter can be made with high accuracy. Errors in the
final results from variations in face angles of indenters
from a reputable supplier are usually negligible. The
reason why a three-sided Berkovich indenter is used in
nanoindentation work over the more familiar Vickers
indenter is that a sharper tip is possible when the indenter
is ground. With a four-sided Vickers pyramid, there is
always an undesirable line of conjunction at the tip. With
a three-sided Berkovich indenter, it is much easier to
grind the faces of the indenter to meet at a single point
than a line. An ideal Berkovich indenter tip has an
infinitely sharp radius, but this is impossible to achieve in
practice. Usually, the tip radius of a new Berkovich
indenter is in the order of 50 –150 nm with an error of
approximately 50% in the estimation. Very small radius
tips are usually obtained from sorting a production batch.
As a result of the finite radius of the indenter tip, it is
necessary to employ contact mechanics equations appro-
priate to a spherical indenter for the initial part of the
loading/unloading cycle, and equations for an equivalent
conical indenter for the higher loading and unloading
portions. To proceed, we first examine the equations of
elastic contact for a spherical indenter.
(b)
θ
hc
 A.C. Fischer-Cripps / Surface & Coatings Technology 200 (2006) 4153 – 4165
3. Contact mechanics
3.1. Loading
Hertz formulated elastic equations of contact for con-
tacting spherical surfaces in the latter part of the 19th
century [6]. The most significant equation from Hertzian
contact mechanics relates the contact radius a to the
combined radius R, the applied load P, and the elastic
properties of the contacting bodies. For the condition
R H a, the Hertz formula is:
3 PR
a3 ¼ : ð1Þ
4 E4
In most cases of interest in nanoindentation testing, the
indenter is in contact with what is essentially a semi-
infinite half space and so R is the radius of the indenter
alone. In like manner, the elastic modulus E* is the
combined elastic modulus of the contacting bodies. In
practice, the indenter is usually made from diamond and
so, for most materials, E* is dominated by the elastic
properties of the specimen. The relationship between the
two is given by:
 2
1 ð 1  v2 Þ 1  v¶ Þ
¼ þ ð2Þ
E4 E E¶
where E¶ and v¶, and E and v, describe the elastic modulus
and Poisson’s ratio of the indenter and the specimen,
respectively. The significance of Eq. (1) is that it may be
expressed in terms of the mean contact pressure, p m, as a
function of the indentation strain, defined as the ratio of
the contact radius a over the indenter radius R:
 
P 4 E4 a
pm ¼ 2 ¼ : ð3Þ
pa 3 p R
The square bracketed terms in Eq. (3) are constants
and so for a completely elastic contact, the mean contact
pressure, or indentation stress, is linearly proportional to
the indentation strain as shown by the solid line in Fig. 2
where the slope is proportional to E*. Consider the
magnitude of the contact stresses, in particular, the shear
stress in the specimen material as load is applied to a
spherical indenter. For a fully elastic response, the
principal shear stress for indentation with a spherical
indenter is a maximum at å 0.47p m at a depth of å 0.5a
beneath the specimen surface directly beneath the indenter
[7]. We may employ either the Tresca or von Mises shear
stress criteria, where plastic flow occurs at s å 0.5Y, where
Y is the material yield stress, to show that plastic
deformation in the specimen beneath a spherical indenter
can be first expected to occur when p m å 1.1Y [8,9]. As
load is further applied, the plastic zone grows in size and
this results in a leveling off of the indentation stress as
shown by the dashed line in Fig. 2. This indicates a
departure from the linear elastic response (Eq. (3)). There
4155
(a) (b)
Elastic
1. R contact
a
Mean contact pressure pm
Transition
2. region
2. 3.
H
Fully-developed
1. plastic zone
3.
Indentation strain a/R
Plastic
zone
Fig. 2. (a) Indentation stress vs. indentation strain for spherical indenter and
(b) schematic of evolution of the plastic zone.
comes a point where any increase in load results in a
proportional increase in the contact radius and so the
mean contact pressure becomes constant (ignoring any
strain hardening effects). Under these conditions of a fully
developed plastic zone, we call the mean contact pressure
the hardness H of the specimen.
It is important to understand that there is a transition
from purely elastic contact to a plastic contact even for a
Berkovich indenter. The relative contribution of the elastic
portion to the shape of the overall load displacement
curve depends upon the indenter tip radius and the yield
strength of the specimen. The sharper the tip, the less the
contribution of the initial elastic response. For an initial
elastic contact, the mean contact pressure increases with
increasing load. At the condition of a fully developed
plastic zone, the mean contact pressure levels off to a
constant value with increasing load and this value of
mean contact pressure is called the hardness. In fact,
hardness, as a material property, is very difficult to define
since it depends on how it is measured. Indentation tests
are very commonly used and so the hardness so obtained
is often called the ‘‘indentation hardness’’ to distinguish it
from other methods that might employ, say, a scratch
technique.
Once the penetration depth becomes larger than the tip
radius, the pyramidal shape of the indenter becomes the
dominant geometrical feature of the indentation. The
contact then usually involves an appreciable amount of
plastic deformation within the specimen. As we shall see,
it is the data taken on the unloading that is used to
determine the area of contact at the maximum load. This
is done by using equations of contact for a conical
indenter where we mathematically transform the actual
pyramidal geometry into an equivalent cone. That is, we
find a cone angle that gives the same area-to-depth ratio
as the actual pyramidal indenter. This can be easily
4156 A.C. Fischer-Cripps / Surface & Coatings Technology 200 (2006) 4153 – 4165

calculated from geometry where for a Berkovich indenter 3.2. Maximum load
of face angle h, we have:
pffiffiffi During an indentation test, as the indenter is loaded into
A ¼ 3 3h2c tan2 h ð4Þ the specimen, the triangular geometry of the Berkovich
indenter eventually dominates any tip-rounding effect and
and for a conical indenter of half-apical angle a we have: the deformation has the property of geometrical similarity.
This means that unless one has an external reference, it is
A ¼ ph2c tan2 a ð5Þ
not possible to set a scale of the deformation since the load,
where h c is the distance as measured vertically from the depth and size of the plastic zone all scale at the same rate.
indenter tip as shown in Fig. 1(b). Equating Eqs. (4) and Contact with a spherical indenter does not have the property
(5) for h = 65.27-, we have a = 70.296- å 70.3-. of geometrical similarity unless it is expressed in terms of
Using the equations of contact for a conical indenter, it is the ratio a/R. Usually, the maximum load is selected so as to
possible, using a reverse analysis of the methods to be be certain that a fully developed plastic zone in the
described below, to predict the shape of the load – displace- specimen material has been achieved.
ment curve even when the contact is fully ‘‘plastic’’ in the At full load, a hold period is often applied to account for
sense of a fully developed plastic zone. It can be shown that, creep effects before the indenter is unloaded. Creep and
assuming a sharp transition from elastic to plastic behaviour, thermal drift in nanoindentation testing are very important
the load –displacement curve, where is the total depth of sources of error and are difficult to distinguish. In both
penetration from the specimen free surface, can be predicted cases, for a constant load hold period, the depth reading may
according to [1]: change. In the case of thermal drift, the depth reading may
" increase (deeper into the specimen) with time or decrease.
rffiffiffiffiffiffi  rffiffiffiffirffiffiffiffiffiffi#2 When creep occurs, the depth reading usually increases.
1 E4 2ð p  2Þ p H
P ¼ E pffiffiffi
4
þ h2 : Thermal drift is not drifting of the electronic signals
ptana H p 4 E4
(although this can happen) but is usually brought about by
ð6Þ changes in the dimension of the contact (indenter, indenter
shaft, and specimen) from thermal expansion or contraction
In this equation, E* is the combined modulus (Eq. (2)),
due to temperature changes. Thermal drift can usually be
H is the hardness (assumed to be constant—i.e. no strain-
minimized by enclosing the apparatus in an insulating
hardening) and a is the equivalent cone angle (70.3- for a
enclosure or waiting a sufficiently long time after handling
Berkovich indenter). The important feature of this equation
to allow thermal equilibrium to be established before
is that the load is related to the square of the displacement.
beginning the test. Creep occurs due to the movement of
The overall shape of the load –displacement curve is shown
material within the specimen under high pressure in the
in Fig. 3.
indentation stress field. In some materials, creep effects may
50 Power law fitting:
slowly dissipate while in others, they may increase as long
B: 193.1034 as the load is applied. The amount of creep can also depend
hr: 0.3085 on the rate of application of load. For materials with a
m: 1.2784 significant amount of creep, it can sometimes be impossible
40 Unloading analysis:
hi : 0.00803 μm to conduct a nanoindentation test in the usual way, and
Pt : 49.73 mN instead, a visco-elastic creep test may be required. For our
ht : 0.65575 μm present purposes, we shall assume that creep and thermal
30 hc : 0.44086 μm
drift issues are not significant and that load is applied quasi-
P (mN)

dP/dh : 183.90 mN/μm

a : 1.2327 μm statically, i.e. the deformation is time-independent.
A : 4.7738 μm2
20 H : 10.4172 GPa
3.3. Unloading
E*(s+i): 72.2778 GPa
E (s) : 75.3504 GPa
After maximum load, or the optional hold period, the
10 applied load is reduced and the resulting penetration depth
recorded. During unloading, there is usually some degree of
elastic recovery of the specimen material as the elastically
0 strained material outside of the plastic zone relaxes and tries
0 0.2 0.4 0.6 0.8 to resume its original shape. This is usually prevented from
h (μm) happening entirely by the presence of the plastic zone which
can be now considered ‘‘dead’’ material. There remains in
Fig. 3. Typical load – displacement curve with a Berkovich indenter on
fused silica at 50 mN. The inset shows values of various quantities of the specimen surface a residual impression. On the load –
interest. (Note: no area correction was applied for the analysis shown in the displacement curve, elastic recovery is evidenced by a
inset). reduction in displacement with decreasing load. For a fully
 A.C. Fischer-Cripps / Surface & Coatings Technology 200 (2006) 4153 – 4165 4157

elastic contact, the unloading curve lies on top of the where a is the radius of the indenter equal to the radius of the
loading curve. For an elastic –plastic contact, the unloading circle of contact and where it should be noted that the depth of
curve is different to the loading curve and the area enclosed penetration is linearly dependent on the load. For this reason,
between them represents the energy lost (as heat) during some instruments prefer to use Eq. (10) rather than Eq. (9) and
plastic deformation. The unloading behaviour is assumed to we shall discuss the significance of this later.
be an entirely elastic affair. That is, even though there is a Referring now to Eq. (9), the derivative of the load P
plastic zone formed, during unloading, this remains ‘‘inert’’ with respect to the displacement h (the contact stiffness) is
and the unloading deformations that do occur are all elastic. given by:
It is assumed that there is no ‘‘reverse’’ plasticity (i.e. no
dP 2E 4 tana
plastic deformation occurring during unloading). It is the ¼2 h: ð11Þ
unloading data that is ultimately used to determine the dh p
radius of the circle of contact and hence the contact area. Substituting into Eq. (9), we have:
The slope of the unloading curve at any point is called the
1 dP
contact stiffness. As will be shown below, the contact P¼ h: ð12Þ
stiffness can be used in conjunction with the calculated 2 dh
contact area to provide a measurement of the combined If the total depth of penetration is h t, at load P t, then as the
elastic modulus of the system. load is removed, the indenter moves through a distance h e as
Treating the contact as an axis-symmetric cone, the shown in Fig. 4.
contact between a rigid conical indenter and an elastic half At P = P t the displacements h r=0 = h e and h r=a = h a . From
space is found from [10]: Eq. (8) at r = a, the plastic (or contact) depth h c is found
pa 4 from:
P¼ E acota; ð7Þ  
2 2ð p  2Þ Pt
hc ¼ ht  ; ð13Þ
where a is the cone semi-angle. The quantity acota is the p dP=dh
depth of penetration h c measured at the circle of contact. where P t and dP/dh are measured during an experiment.
The depth beneath the specimen free surface within the The square-bracketed term in Eq. (13) is often given the
circle of contact is given by: symbol e and evaluates to 0.72 but it is common practice to
p r use a value of 0.75 since this has been shown to account for
h¼  acota r V a: ð8Þ non-uniformities in the material response as the load is
2 a
withdrawn. Once a value for h c has been determined, the
With r = 0, and substituting into Eq. (7), we obtain: area of contact is found from Eq. (5) where, for a Berkovich
4  indenter (a = 70.3-), Eq. (5) evaluates to:
2E
P¼ tana h2 ; ð9Þ
p A ¼ 24:5h2c : ð14Þ
where the load is proportional to the square of the The reduced elastic modulus is found from [11]:
penetration depth. Eq. (9) should be compared with Eq. pffiffiffi
(6) where it can be seen that for the case of a conical dP 1 p
E ¼
4
p ffiffiffi : ð15Þ
indenter, the square relationship between the load and the dh 2 A
depth features in both cases, although with different Experiments and finite element analysis shows that a
constants of proportionality. correction factor is needed for Eq. (15). The correction
For the case of the unloading data in a nanoindentation
test, we consider the contact conditions at this point to be
entirely elastic. That is, we can unload and reload as many a
times as we like and travel down and up the unloading curve
ha
without any further plastic deformation taking place. unloaded
Experiments show that in nearly all cases, reloading the
residual impression to the same maximum load does indeed
take place up the unloading curve implying that the hf
unloading and the reloading is elastic. So, the unloading
ht
curve can be treated as if it were an elastic loading hc
according to Eq. (6). Historically, it was noted that the he α
initial unloading response for many materials was linear.
This implied that the contact conditions were those of a loaded
cylindrical punch instead of a cone where:
Fig. 4. Cross-section of profile of specimen surface at full load, and full
P ¼ 2aE 4 h; ð10Þ unload for an elastic – plastic indentation. Symbols are defined in the text.
4158 A.C. Fischer-Cripps / Surface & Coatings Technology 200 (2006) 4153 – 4165
factor is given the symbol b and is applied as the factor 1/b
to the measured value of dP/dh. Accordingly we have:
pffiffiffi
1 dP 1 p
E ¼
4
pffiffiffi ð16Þ
b dh 2 A
and
Pt
hc ¼ ht  eb ð17Þ
dP=dh
where dP/dh in Eqs. (16) and (17) is that as actually
measured from the experimental data. King [12] performed
finite element calculations for elastic indentations formed
with flat-ended punches of triangular and circular cross-
sections and found b = 1.034. Dao et al. [13] determined
b = 1.096 for a Berkovich indenter and b = 1.0595 for a
70.3- conical indenter from a 3D elastic – plastic finite
element analysis (note that 1.096/1.0595 = 1.034). Cheng
and Cheng [14] determined, on the basis of elastic – plastic
finite element calculations with a 68- conical indenter at
v = 0.3, that b = 1.05 for non-work-hardened materials.
Larsson et al. [15] estimated b = 1.14 on the basis of a 3D
elastic solution for a Berkovich indenter using the finite
element method. Hay et al. [16] calculated b = 1.067 on the
basis of radial displacements within the circle of contact for
an elastic contact with a conical indenter (a = 70.3- and
v = 0.3) from finite element results. Borodich and Keer [17]
proposed b = 1.058 (at v = 0.17) on theoretical grounds for
full adhesive (non-slip) contact for a conical indenter.
Martin and Troyon [18] measured b = 1.063 experimentally
with a Berkovich indenter. Gong et al. [19] evaluated
b = 1.032 from experimental results involving a consider-
ation of the presence of the residual stress field on the
unloading response. In carefully considering the above, it
appears that the factor 1.034 reasonably represents the
change from axis-symmetric to a pyramidal cross-section
while an additional factor å 1.06 is required on the basis of
a variety of causes ranging from radial displacements to
interfacial friction. The product of the two gives 1.09. A
similar survey was conducted by Oliver and Pharr [5] who
suggested a value of 1.05 as a reasonable estimate.
Evidently, the factor b should be greater than the commonly
used 1.034 but at present there appears to be no consensus
as to why the factor arises and what value it should take.
4. Fitting the load – displacement curve
We are now in a position to analyse the experimental
data in the form of a load – displacement curve. In its most
basic form, the curve consists of a quasi-static loading to
full load followed by an unloading to zero load. From the
point of view of the analysis equations given above, it is
the initial unloading data that is the most significant
although we shall see that the other data also is of
considerable importance.
In the derivation given in Section 3, it can be seen that to
determine the contact depth h c, we need to evaluate the
contact stiffness dP/dh at full load P t. This is usually done
by fitting an equation to the unloading data, then finding the
derivative of that equation which gives the contact stiffness
dP/dh. If the data were to satisfy Eq. (6), then all we would
need to do is to fit a polynomial expression of the 2nd
degree to the data, perhaps using a least squares approach,
and then find the derivative and the slope.
Here is where we return to the significance of Eq. (10).
Initially, it was noticed that the unloading response, at
least for the initial part, was fairly linear. This means that
instead of a 2nd order polynomial (Eq. (9)), the contact
appeared to have a linear dependence on the load as if the
indenter were a cylindrical punch (as per Eq. (10)). For
some materials, the initial unloading data is indeed almost
linear and a linear fit to the upper portion of the
unloading data is entirely reasonable. However, for other
materials, particularly those with a relatively large amount
of elastic recovery (low value of the ratio E/H), the
unloading data was observed to be curved, but more than
would be expected on the basis of a conical indenter (Eq.
(9)). In most cases, a 2nd degree polynomial fit to the
unloading data provides a reasonable fit to the data, but
for best results, a power law fit is appropriate. For a
power law fit, we fit the data using:
P ¼ Bðh  hf Þm ð18Þ
where m is the power law index, B is a constant, and h f
is the final residual depth measured from the original
specimen free surface, all of which are unknown
quantities. Fitting can only be done using an iterative
procedure (see Appendix 4 in Ref. [1]). The fitting
procedure relies on there being an initial guess for B, m
and h f, all of which can be obtained by an initial 2nd
degree fit. The iterative procedure then provides the best
fit values for these unknowns based upon a least squares
approach.
When a power law fitting is done, it is found that the
index m ranges from 1.1 to 1.8 depending on the specimen
material. The reason for the index not being precisely equal
to 2 appears to be due to that fact that the contact described
by Eq. (9) assumes that the notional conical indenter is in
contact with a conical residual impression. The presumption
is, and this is not often appreciated, that the specimen
material elastically recovers so that the sides of the residual
impression remain straight. This is essentially the origin of
the factor 2 in Eq. (13). Careful measurement with an AFM
and finite element analysis shows that the sides of the
residual impression are usually curved upwards. According
to Pharr and Bolshakov [20], this results in contact actually
occurring between a notional elastic half space and an
indenter with an arbitrary shape that provides the necessary
observed unloading response. Thus, we need not be too
concerned about the actual shape of the effective indenter
because it is embodied in the power law index m in Eq. (18).
 A.C. Fischer-Cripps / Surface & Coatings Technology 200 (2006) 4153 – 4165
The notion of the effective shape of the indenter also
accounts for the commonly used choice of e = 0.75 [20].
The analysis procedure given above is often called the
‘‘Oliver and Pharr’’ method after the authors who gave it
particular study [21]. Some practitioners often misapply the
Oliver and Pharr method by using a linear fit to the
unloading data, using a polynomial fit (2nd degree) without
actually checking to see if the fitted line corresponds to the
actual experimental data or using a power law fit but instead
of finding values of B, h f and m from the data, use values
verbatim from Oliver and Pharr’s paper. In most cases, the
resulting errors are not large because it is the initial
unloading data that is usually used for the fitting. However,
the recent ISO standard on instrumented indentation testing
[22] recommends using 80% of the unloading data in which
case the fitting procedure becomes very important. The
reason for using the initial part of the unloading data stems
from Doerner and Nix [23] who wished to only use the
observed linear portion of the data and Eq. (10). If a power
law fit is used, it is perhaps more appropriate to use a greater
proportion of the unloading data so as to obtain a more
precise fit as suggested in ISO 14577. Because the contact
stiffness is evaluated at the maximum load, there is a large
‘‘leverage’’ effect which magnifies errors in determining the
contact depth from Eq. (13). Errors in the quantity dP/dh
affect the computed value of h c. Since the area of contact
depends on h c2 (Eq. (14)), the error in the calculated area will
be twice the percentage error in h c.
5. Corrections
As mentioned previously, it is necessary in most nano-
indentation testing to account for various sources of error in
the instrumented data before arriving at a final value for
modulus and hardness of the test specimen. Three of the
most common, and necessary corrections are the initial
penetration, the instrument frame compliance, and the
indenter area function. There are also some materials-related
issues which are also important but more difficult to correct
for, the main ones being the presence of indentation size
effects, and piling-up of material around the indentation.
5.1. Initial penetration or zero point determination
A very important procedure in nanoindentation testing is
the determination of the initial contact between the indenter
and the specimen. This is important because the contact
point determines the datum of the displacement measure-
ment. There are a variety of ways in which the contact point
is estimated. In one method, the force and depth signals are
constantly monitored at a rapid rate and the software or the
operator determines the point of contact from a sharp rise in
the force data. In another method, an initial contact force, set
by the user, is commanded, and once achieved, the depth
sensor is then set to zero and the loading then proceeds.
4159
Afterwards, a smooth curve is fitted to the initial data and
then extrapolated back to zero force. This provides a
measure of the initial contact depth which is then added
on to all the subsequent depth readings. The initial
penetration correction has the effect of shifting the load –
displacement curve to the right as shown in Fig. 5.
The initial penetration h i is applied to all the displace-
ment readings to give a corrected depth of penetration.
h¶ ¼ h þ hi ð19Þ
where h¶ is the corrected value of the penetration depth and
h is the depth recorded by the instrument. The significance
of the initial penetration correction depends upon the
magnitude of the maximum load applied to the indenter
relative to the magnitude of the initial contact force. The
lowest force that can be detected or set in a typical
nanoindenter is in the order of 2– 5 AN. Typically, the
initial penetration is a few nanometers. For a typical
maximum load of over 10 mN in a moderately hard and
stiff material, the initial penetration correction will make a
few percent difference to the computed values of E and H.
5.2. Frame compliance
Frame compliance is the contribution to the depth
readings arising from deflections of the load frame instead
of displacement into the specimen material. When load is
applied, the reaction force is taken up by deflection of the
load frame and it is this deflection that is typically added to
the depth readings. The deflection is usually linearly
proportional to the applied load in the manner of a linear
spring.
The correction takes the form of the product of the
known instrument compliance C f and the force P and is
subtracted from the depth reading as recorded by the
4
3
P (mN)
2
1
0
-0.05 0 0.05 0.1 0.15 0.2
h (μm)
hi
Fig. 5. Initial penetration h i is estimated by extrapolating the recorded
load – displacement data back to zero load.
4160 A.C. Fischer-Cripps / Surface & Coatings Technology 200 (2006) 4153 – 4165
instrument (note, the initial penetration correction should be
applied first):
h¶ ¼ h  PCf : ð20Þ
The effect of the compliance correction is to shift the
load –displacement curve to the left, somewhat negating
the effect of the initial penetration correction. However, the
compliance correction is dependent on the load and is not
a constant (as is the initial penetration correction) so it is
not possible to completely balance the two effects over the
whole load range of the test. The compliance correction is
particularly important when testing very stiff materials. In
this case, the contribution to the depth signals from the
frame compliance is a greater proportion of the overall
signal. If not correctly applied, the compliance correction
can make up to a 50% difference in the resulting
estimations for modulus and hardness.
The compliance correction obviously requires a knowl-
edge of the value of C f. Often, this is measured by the
instrument manufacturer and is set internally within the
software. While this might provide some measure of
correction, trusting this value can lead to significant
problems. In particular, it should be noted that the factor
C f contains all the compliances of the system which are
linearly dependent upon the applied force. These com-
pliances are those of the load frame, the indenter shaft
and (and what is often overlooked) the specimen
mounting. A common mistake is to mount the specimen
using a thick layer of mounting resin which itself is quite
compliant and may not be accounted for by the
manufacturer’s figure for C f. The best way to measure
and verify the value of C f is to conduct a series of tests at
different loads on a fairly stiff specimen (e.g. sapphire).
The contact stiffness dP/dh as measured by the instrument
actually consists of the actual stiffness of the contact at
the indenter, given the symbol S, and the reciprocal of the
instrument compliance C f. Expressed in terms of com-
pliances, we have:
dh 1
¼ þ Cf : ð21Þ
dP S
Interpreting Eq. (21) in terms of the analysis method
given above, we have:
"rffiffiffiffiffiffiffiffiffi #
dh p 1 1 of measuring indenter penetration. In this method, the
¼ þ Cf ð22Þ
dP 24:5 2E4 hc
where we can see that a plot of dh/dP vs. 1/h c gives a
straight line with an intercept C f. Fig. 6 shows such a plot
with real data taken on sapphire with a Berkovich
indenter. Note that the data at the higher end of the
range arises from load – displacement data at the low end
of the depth measurement and has a greater error
associated with it. In some cases, it may be necessary
0.003
0.002
dh/dP
0.001
0
0 2 4 6 8
1/hc
Fig. 6. Plot of dP/dh vs. 1/h c for data taken on sapphire over a load
range of 20 mN to 100 mN A linear fit to the data gave an intercept
C f = 0.00014 Am/mN.
to give more weight to the data from the higher end of
the load range in determining the value of C f.
A common mistake in operating or calibrating a
nanoindentation instrument is to determine the compli-
ance C f using only one reference standard. For example,
it is common practice to use fused silica to determine the
area function (see Section 5.3) of the indenter and to also
estimate the compliance correction. What is not often
appreciated is that the two procedures are inextricably
linked so that one may indeed arrive at a value of C f and
an area function which gives perfectly good results for
tests on materials with a similar value of modulus and
hardness as the reference specimen, but may give very
poor results for harder and stiffer materials. For best
results, one should determine the C f on a variety of
standard specimens (fused silica, silicon and sapphire
provide a very good range) and make sure that the value
of C f is consistent for each. The area function should
also be calculated using the new value of C f and then C f
re-evaluated until there is a convergence to a fairly
constant value. This does not mean that tests on the
standard specimen should be repeated until convergence
is obtained, but simply re-analysed.
In some instruments, compliance corrections are
eliminated, or nearly so, by using a differential method
depth sensor datum is located on a reference ring which
typically advances ahead of the indenter and makes
contact with the specimen surface outside the prospective
indentation site. This arrangement also serves to minimize
thermal drift errors. The disadvantage is that the method
is restricted to relatively hard materials (lest the reference
ring sink into the specimen or the force applied to the
reference ring causes unwanted local deformations in the
specimen surface).
 A.C. Fischer-Cripps / Surface & Coatings Technology 200 (2006) 4153 – 4165
10
8 geometry. Eq. (23), flexible as it might seem, ignores the
6 geometry, or conversely, use of such an equation might
A/Ai
4
2 indenter shape. The issue is very important since even small
0 present author’s experience that fitting equations such as
0 0.4 0.8 1.2 1.6
hc (μm)
Fig. 7. Area function for a Berkovich indenter expressed in terms of the
ratio A/A i vs. h c where A i is the ideal area of contact for a perfect indenter.
Convergence to A/A i = 1 at large values of h c indicates that the face angles
of the indenter are correct. The sharp rise in the value of A/A i at low values
of h c indicates tip rounding.
5.3. Area function
The area function of the indenter is a function or a table
of values that provides the best estimate of the area of
contact as a function of the contact depth for the indenter
being used. As mentioned previously, indenters are usually
made with high precision and accuracy with regard to the
face angles, but the ideal geometry often breaks down near
the very tip where tip rounding has occurred (either through
use of the indenter or just from the manufacturing process).
The area function can be found using a variety of methods.
An independent measure using an AFM or similar profiling
instrument may be beneficial but is usually very inconven-
ient. It is more common to test a material of known modulus
(or hardness) and to use Eq. (15) to determine the value of A
as a function of h c over the load range of the instrument.
This procedure usually results in a range of data points to
which a smoothing equation can be applied.
In many cases, the area function equation takes the form:
A ¼ C1 h2c þ C2 hc þ C3 h1=2 1=4
c þ C 4 hc þ N ð23Þ
where C 1 is usually a number close to 24.5 and the
remaining fitting constants account for the tip rounding and
other departures from the ideal shape. For example, Fig. 7
shows a typical area function for a new Berkovich indenter.
There is evidently some scatter in the data, particularly (and
expectedly) at the lower end of the load range. This scatter
arises from instrument errors (particularly near the low end
of the instrument range), surface roughness, and irregu-
larities in the indenter. Should one then smooth out this
scatter using an equation such as Eq. (23) above? While it is
tempting to express area function equations in terms of
physically meaningful parameters in equations such as Eq.
4161
(23) (e.g. terms that correspond to tip rounding and indenter
face angle), such attempts tend to ignore local variations in
fact that such local irregularities are unlikely to present
themselves at regular harmonic intervals in the indenter
introduce irregularities of a harmonic nature where none are
justified. That is, it depends on whether the scatter in Fig. 7
represents the real irregular shape of the indenter or is a
result of some other cause not associated with the actual
errors in the area function make a significant difference to
the final results obtained with the instrument. It is the
that above lead to systematic errors over the load range of
the instrument since the fitting is never perfect over this
range. It is far better to smooth out some of the data using a
running average which retains any short to medium length
scale deviations in the shape of the indenter while
smoothing out small length scale irregularities from surface
roughness of the standard reference specimen.
When establishing an area function, it is important to do
so over the whole load range of the instrument. If
measurements are to be taken at relatively low loads, then
more data points should be taken at the low end of the load
range, giving particular attention to the point at which the
area function ratio shows a sharp increase. In Fig. 7, the
results from four separate indentation tests were combined
to form a single area function for the indenter which covered
penetration depths up to about 2 Am.
5.4. Materials issues
Even if the corrections listed above are attended to,
there remain various materials-related effects which can
cause errors in the estimation of modulus and hardness of
the test specimen. The most significant of these materials
issues is that of piling-up. To understand what piling-up
is, it is necessary to be aware of the opposite effect of
sinking-in. Fig. 4 shows a cross-section of the profile of
the specimen surface under full load. It is evident that the
circle of contact lies below the specimen free surface. A
certain amount of sinking-in of the surface is expected,
even for a purely elastic contact. For a contact involving
Sinking-in Piling-up
a
a
hc
ht
hc
Fig. 8. Schematic of piling-up compared to sinking-in.
4162 A.C. Fischer-Cripps / Surface & Coatings Technology 200 (2006) 4153 – 4165
plastic deformation, there is the possibility of the surface
actually being raised up at the edge of the indentation as
illustrated in Fig. 8.
When piling-up does occur (as if often the case with
indentation testing of metals), the material which has
piled-up supports the load applied to the indenter and so
the indenter penetrates less compared to the case where
there is no piling-up. However, the analysis method
discussed in Section 3.3 does not take this into account
and so the material appears to be stiffer and harder. The
area of contact A, computed from the combination of Eqs.
(15) and (18), is less than the actual area and so both E
and H are over-estimated. These over-estimates can be
quite substantial, up to 50% in some cases. The only
satisfactory method to eliminate this error is to measure
the area of contact directly. An AFM image is probably
the most convenient, but even so, requires considerable
capital outlay and investment in time. There are some
analytical [24,25] treatments which deal with piling-up but
these generally apply to particular materials system.
What is not often appreciated is that piling-up need not
actually be described by h c > h t. Any increase in the value
of h c over that which is expected by the equations of
contact used in the unloading analysis represents a piling-
up even if h c < h t. Further, the amount of piling-up for
even nominally brittle materials may take place if the
loading is high enough. For example, Fig. 9 shows piling-
up in an impression in fused silica with a 70.3- conical
indenter under a load of 175 mN. Piling-up is perhaps the
most important unresolved issue in nanoindentation test-
ing. There are two ways to approach the problem: (i)
perform an area function calibration on a reference
specimen which has a similar ratio of E/H as the test
specimen (such that piling-up is accommodated within the
area function correction) or (ii) ignore the effect and treat
the resulting values of E and H as comparative values.
Although (ii) may sound somewhat unsatisfactory, that is
precisely what is implicitly recommended by ISO 14577
in the labeling of the quantities as the ‘‘indentation
modulus’’ and the ‘‘indentation hardness’’.
8 μm
Fig. 9. AFM scan of a residual impression in fused silica after indentation
with a 70.3- conical indenter at 175 mN. Piling-up is in evidence around the
edge of the impression.
6. Interpretation of the results
Assuming now we have made the necessary corrections
and obtained values of the reduced modulus and hardness, it
is now required that we correctly interpret the data. The
following discussion is directed towards the testing of thin
films but some of the issues are applicable to tests on bulk
specimens. Of particular interest in the testing of thin films
is the well-known 10% rule. This rule states that in order to
minimize the effect of the substrate properties of the
measurement of the film properties, the indentation depth
should be no more than 10% of the film thickness. This
widely quoted and often misused rule has its basis in the
determination of hardness testing where the intention was to
restrict the extent of the plastic zone to the film material.
Common practice has transferred the rule to the determi-
nation of modulus although there is no real physical basis to
support its use for that purpose.
6.1. Elastic modulus
When testing a thin film deposited on a substrate using
an indentation technique, most of the deformation is
localized to the vicinity of the indenter and so we can
ignore any large-scale bending or compression of the
specimen (or hope that these deformations are accommo-
dated by the compliance correction). The indentation stress
field is a complex mixture of biaxial stresses, there being
elements of tension, compression and shear. In the simplest
treatment, we can imagine that the indenter bears down on
an elastic film that in turn is connected to an elastic
substrate. The reaction force is thus supplied by a linear
combination of two springs in series. Of course, in reality,
the reaction force is supplied by material within the film
acting radially inwards from many directions and not simply
in the vertical direction, but the simple linear model does
reinforce the important result that the elastic modulus so
measured, no matter how small the penetration depth, is a
combined modulus of the film and substrate system. The
task then is to separate out the substrate modulus (or
compliance) so that we are left with a measurement of the
modulus of the film. There are several methods by which
this is done.
The simplest method involves taking a series of
indentations over a range of loads and then plotting the
elastic modulus as a function of penetration depth. It is
necessary to obtain a sufficient number of data points at low
loads so that the data near the lower end of the depth axis
captures, as much as possible, the film properties. Once
obtained and plotted, a smooth curve is fitted to the data and
extrapolated back to zero depth (where there is of course no
data point) as shown in Fig. 10. The vertical axis intercept is
then taken as the best estimate of the film modulus. Simple
as it is, the method can provide inaccurate results for the
unwary because it assumes that the error in the area function
used to analyse the data is small, even at very small
 A.C. Fischer-Cripps / Surface & Coatings Technology 200 (2006) 4153 – 4165 4163

600 I o is in effect a weighting function that equals zero as the

film thickness approaches zero, and approaches unity for
Ef
large values of film thickness. A simpler approach is given
500 by Jung et al. [27] who propose an empirical power law
relationship:
E (GPa)

L
400 Ef
Ec ¼ Es þ ; ð27Þ
Es
ES
300 where
1
L¼ ; ð28Þ
200
1 þ Aðh=t ÞC
0 0.2 0.4 0.6 0.8 1 where the constants A and C are found a best-fit analysis of
ht (μm) the data. More formal treatments involving numerical
solutions of complex exact analytical functions are given
Fig. 10. Estimation of elastic modulus of super-hard site nc-TiN/a-BN film
by Stone [28], Yoder et al. [29], Schwarzer [30], Chuboba et
(5 Am thick) on a steel substrate using the extrapolation technique. At large
indentation depths, the combined modulus tends towards the substrate al. [31], and also Perriot and Barthel [32].
modulus E S. Extrapolation of the data to zero depth provides an estimate of As a first order approximation, the extrapolation techni-
the film modulus E f. que provides a readily accessible method for determining
the film-only modulus. Where data cannot be easily treated
penetrations. Consider the area function shown in Fig. 7. in this way, a simple empirical approach such as that given
Evidently, any estimates of modulus at depths of penetration in Eq. (27) is probably the next best method. Where the
below about 150 nm will result in the area function ratio situation is complicated by a large mismatch in properties
being taken on the steeply rising part of the curve where the between film and substrate, or the film is very thin, then the
error in the estimation of the ratio will be very high. One more formal treatments are appropriate. It should be noted
should then treat the modulus data at these depths with some in closing this section that a sharp tip indenter is not
caution. It is easy for the plot of modulus vs. depth to be just required for a measurement of elastic modulus. Indeed, a
reflecting the shape of errors in the area function rather than spherical indenter may be more beneficial since the area
any real trends in the film properties. A better approach function data at small penetration depths will not be so
would be to perform this estimation for a range of sharply rising (as in Fig. 7) and so the associated errors in
specimens of different thickness and perhaps even on the estimation of the contact areas will be likely to be much
different substrates. smaller.
As an alternative to the above procedure, we may
recognize from the outset the combined nature of the elastic 6.2. Hardness
modulus values and attempt to fit a suitable constitutive
equation to determine the film modulus on its own. There Assuming then that we have a very sharp Berkovich tip,
are a variety of treatments available. For example, King [12] how then is the hardness of the film determined? The 10%
used the finite element method to obtain the combined rule provides a reasonable starting point. The assumption
modulus of the film of thickness t and substrate E c: behind the rule is that if the total depth of penetration of the
 
1 1  v2f Þ  pffiffiffi 
at= A 1  v2s Þ  at=pffiffiAffi  indenter is less than 10% of the film thickness, then the
¼ 1e þ e plastic zone associated with the indentation will be
Ec Ef Es
contained entirely within the film and there will be a
 2
1  v¶ Þ negligible contribution from any elastic deformation of the
þ ; ð24Þ substrate. This is a somewhat simplified assumption but one
E¶
where a is an empirical constant. Gao et al. [26] proposed: that may provide reasonable values in many cases,
especially when the film is not too thin and the indenter
Ec ¼ Es þ ðEf  Es ÞIo ; ð25Þ not too blunt.
where I o is a function of t/a (where a is the contact radius) A slightly better approach is to perform a series of
given by: indentations at increasing depths of penetration and then
"  plotting the calculated hardness against depth. Much like the
2 1 t t ðt=aÞ2 extrapolation technique for modulus in the previous section,
Io ¼ tan þ ð1  2vÞ ln 1 þ
p a a ðt=aÞ2 we draw a smooth curve through the data. Fig. 11 shows
  data obtained on a super-hard nc-TiN/a-BN film.
t=a 1
 2
: ð26Þ There are several points of interest to be noted in Fig. 11.
1 þ ðt=aÞ 2p ð 1  vÞ The initial rise in hardness at low penetration depths is
4164 A.C. Fischer-Cripps / Surface & Coatings Technology 200 (2006) 4153 – 4165

60
More formal methods of estimating the film-only hard-
ness rely on mathematical modeling of the film – substrate
system. As far back as 1973, Bückle [33] proposed that the
50 composite hardness of a thin film/substrate system H c could
be found from:
H (GPa)

Hc ¼ Hs þ aðHf  Hs Þ; ð29Þ
40
where H s is the hardness of the substrate and H f is the
hardness of the film. In this equation, a is an empirically
derived parameter. Jonsson and Hogmark [34] propose an
30 area law of mixtures such that:
Af As
Hc ¼ Hf þ Hs ; ð30Þ
A A
20
0 0.2 0.4 0.6 0.8 1 where A f and A s are the relative parts of the contact area
ht (μm) carried by the film and the substrate, respectively, and A is
the total contact area. A similar treatment, but based on a
Fig. 11. Measured hardness of a super-hard nano-composite nc-TiN/a-BN volume of deformation law of mixtures, was proposed by
film (5 Am thick) on a steel substrate. Three regimes, initial rise, plateau and Burnett and Rickerby [35,36]:
fall-off can be identified.
Vf Vs
Hc ¼ Hf þ Hs : ð31Þ
V V
usually, but mistakenly, ascribed on an indentation size
effect (ISE), the details of which are usually not divulged. In For a soft film on a hard substrate, Bhattacharya and Nix
fact, an initial rise in hardness, in most cases and especially [37] propose that the combined hardness is determined by:
in very hard materials, is entirely expected on the grounds  !
Yf Es h 2
that the indenter tip, at this scale of testing, is initially round Hc ¼ Hs þ ðHf  Hs Þexp  ; ð32Þ
and so the contact is elastic. The value of hardness Ys Ef t
calculated under these conditions is the mean contact where Y f and Y s are the material yield stresses for the film
pressure, which, for a given load, will be less than the and substrate, respectively, and the exponential is a
hardness of the specimen material. Once we have a fully weighting function. For hard films on a soft substrate, the
developed plastic zone, the hardness of the film should expression becomes:
reach a constant or plateau. At larger loads, or greater rffiffiffiffiffiffi 
depths, the influence of the substrate will then be felt and Hf Ys Es h
Hc ¼ Hs þ ðHf  Hs Þexp  : ð33Þ
the hardness may increase or decrease according to the Hs Yf Ef t
relative hardness of the film and substrate. It is important to
use the sharpest possible tip when one desires to measure Many other models attempt to correlate the combined or
the hardness of a very thin film. If the indenter is too blunt, effective hardness with the hardness of the individual
then most of the deformation may be elastic and the mean components [27,38 – 40]. Given so many treatments, which
contact pressure so measured will not reflect the film should be chosen? In most practical situations, if the film is
hardness. thick enough and the indenter sharp enough, the simple
The identification of these three regimes of hardness extrapolation technique is probably the most straight-
(initial rise, plateau, and falling-off or increase) are forward and accessible. The analytical treatments require a
important validity checks on the data so obtained and certain sense of ‘‘calibration’’ on specimens of known
quoted for the film-only hardness. (a) Should there be no hardness. However, the advantage of these techniques is that
initial rise, the cause should be investigated. It is unlikely the hardness of films on substrates whose properties are not
that the indenter is infinitely sharp. More likely, the load known may be measured.
applied is too large and the indenter has gone through to
the substrate without providing any data points for the
film. (b) Should there be no plateau region, then it is 7. Conclusion
likely that the indenter is too blunt and so a fully
developed plastic zone could not be established before it The present paper seeks to clarify the issues involved in
extended into the substrate. (c) Should there be no the analysis of nanoindentation test data so that practitioners
obvious fall-off or increase in hardness at large pene- may avoid common mistakes made in the analysis and
tration depths, then perhaps the film and substrate have presentation of their data. Common mistakes are the failure
similar mechanical properties or the film is very thick to recognize the initial rise in hardness as resulting from
relative to the maximum indentation depth. elastic contact from the rounded tip of the indenter,
 A.C. Fischer-Cripps / Surface & Coatings Technology 200 (2006) 4153 – 4165
improper fitting of the area function data, failure to account
for instrument compliance or check that the instrument
compliance is independent of the sample being tested, not
fitting the unloading data with an iterative technique or
selecting too many data points when using a polynomial or
linear fitting, failure to account for piling-up, and failure to
correctly determine the film-only modulus and hardness by
insufficiently spaced data. All these issues can have a
significant effect on the quality of the data presented and
also their interpretation.
Acknowledgement
The author is indebted to Martin Soh for interesting
discussions on the issues discussed in this paper.
References
[1] A.C. Fischer-Cripps, Nanoindentation, 2nd edR, Springer-Verlag, N-Y,
2004.
[2] A.C. Fischer-Cripps, Vacuum 58 (4) (2000) 569.
[3] J.L. Hay, G.M. Pharr, ASM Handbook, Materials Testing and
Evaluation, vol. 8, 2000, p. 232.
[4] Y. Gogotsi, V. Domnich (Eds.), High Pressure Surface Science and
Engineering, Institute of Physics, Bristol, UK, 2004.
[5] W.C. Oliver, G.M. Pharr, J. Mater. Res. 19 (1) (2004) 3.
[6] H. Hertz, J. Reine Angew. Math. 92 (1881) 156 (Translated and
reprinted in English in Hertz’s Miscellaneous Papers, Macmillan and
Co., London (1896) Ch. 5).
[7] M.T. Huber, Ann. Phys. 14 (1) (1904) 153.
[8] D. Tabor, The Hardness of Metals, Clarendon Press, Oxford, 1951.
[9] K.L. Johnson, Contact Mechanics, Cambridge University Press,
Cambridge, 1985.
[10] I.N. Sneddon, Proc. Camb. Philos. Soc. 44 (1948) 492.
[11] G.M. Pharr, W.C. Oliver, F.R. Brotzen, J. Mater. Res. 7 (3) (1992) 613.
[12] R.B. King, Int. J. Solids Struct. 23 (12) (1987) 1657.
4165
[13] M. Dao, N. Chollacoop, K.J. Van Vliet, T.A. Venkatesh, S. Suresh,
Acta Mater. 49 (2001) 3899.
[14] Y.-T. Cheng, C.-M. Cheng, J. Appl. Phys. 84 (3) (1998) 1284.
[15] P.-L. Larsson, A.E. Giannakopoulos, E. Soderlund, D.J. Rowcliffe, R.
Vestergaard, Int. J. Solids Struct. 33 (2) (1996) 221.
[16] J.C. Hay, A. Bolshakov, G.M. Pharr, J. Mater. Res. 14 (6) (1999)
2296.
[17] F.M. Borodich, L.M. Keer, Proc. R. Soc. Lond., A 460 (2004) 507.
[18] M. Martin, M. Troyon, J. Mater. Res. 17 (9) (2002) 2227.
[19] J. Gong, H. Miao, Z. Peng, Acta Mater. 52 (2004) 785.
[20] G.M. Pharr, A. Bolshakov, J. Mater. Res. 17 (10) (2002) 2660.
[21] W.C. Oliver, G.M. Pharr, J. Mater. Res. 7 (4) (1992) 1564.
[22] ISO 14577, Metallic materials—Instrumented indentation test for
hardness and materials parameters, ISO Central Secretariat, 1 rue de
Varembé, 1211 Geneva 20 Switzerland.
[23] M.F. Doerner, W.D. Nix, J. Mater. Res. 1 (4) (1986) 601.
[24] K.W. McElhaney, J.J. Vlassak, W.D. Nix, J. Mater. Res. 13 (5) (1998)
1300.
[25] A. Bolshakov, G.M. Pharr, J. Mater. Res. 13 (4) (1998) 1049.
[26] H. Gao, C.-H. Chiu, J. Lee, Int. J. Solids Struct. 29 (20) (1992) 2471.
[27] Y.-G. Jung, B.R. Lawn, M. Martyniuk, H. Huang, X.Z. Hu, J. Mater.
Res. 19 (10) (2004) 1.
[28] D.S. Stone, J. Mater. Res. 13 (11) (1998) 3207.
[29] K.B. Yoder, D.S. Stone, R.A. Hoffman, J.C. Lin, J. Mater. Res. 13 (11)
(1998) 3214.
[30] N. Schwarzer, ASME J. Tribol. 122 (4) (2000) 672.
[31] T. Chudoba, N. Schwarzer, F. Richter, Thin Solid Films 355 – 356
(1999) 284.
[32] A. Perriot, E. Barthel, J. Mater. Res. 10 (2) (2004) 600.
[33] H. Bückle, in: J.W. Westbrook, H. Conrad (Eds.), The Science of
Hardness Testing and its Applications, American Society for Metals,
Metals Park, OH, 1973, p. 453.
[34] B. Jonsson, S. Hogmark, Thin Solid Films 114 (1984) 257.
[35] P.J. Burnett, D.S. Rickerby, Thin Solid Films 148 (1987) 41.
[36] P.J. Burnett, D.S. Rickerby, Thin Solid Films 148 (1987) 51.
[37] A.K. Bhattacharya, W.D. Nix, Int. J. Solids Struct. 24 (12) (1988)
1287.
[38] S.J. Bull, Mater. Res. Symp. Proc. 750 (2003) Y6.1.1.
[39] A.M. Korunsky, M.R. McGurk, S.J. Bull, T.F. Page, Surf. Coat.
Technol. 99 (1998) 171.
[40] E.S. Puchi-Cabrera, J.A. Berrios, D.G. Teer, Surf. Coat. Technol. 157
(2002) 185.