Measuring Methods and Applications of Nanoindentation

CIRP Annals - Manufacturing Technology 59 (2010) 803819
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CIRP Annals - Manufacturing Technology

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Nanoindentation: Measuring methods and applications

D.A. Lucca (1)a,*, K. Herrmann b, M.J. Klopfstein c
a
b
c
School of Mechanical and Aerospace Engineering, Oklahoma State University, Stillwater, OK, USA
Physikalisch-Technische Bundesanstalt, Braunschweig, Germany
Laboratory for Precision Machining (LFM), Bremen, Germany
A R T I C L E I N F O
A B S T R A C T
Keywords:
Surface
Nanoindentation
Mechanical property
Nanoindentation has emerged as an important method for the evaluation of the mechanical response of
small material volumes and thin lms to applied loading. Here, we present a review of the measurement
method, the instruments currently in use and the procedures for the analysis of the resulting data. The
methods developed for verication and calibration, including a discussion on uncertainty of parameters
are presented. The results of the most recent CIRP sponsored comparison on nanoindentation are
presented and compared to the results obtained in the rst such comparison. Examples of some of the
emerging uses of the technique are included.
2010 CIRP.
1. Introduction
century, instruments which measured indentation depth under

low load emerged. These are reported in the early work of
Grodzinski [2] in 1953 and then in the 1970s in the works of
Alekhin et al. [3,4], Ternovskij et al. [5] and Bulychev et al. [6] in the
former Soviet Union, of Kinosita et al. [7,8] in Japan, and of Frohlich
et al. [9,10] in the GDR. The work of Ternovskij and colleagues
described the force-indentation depth curve and a method for
deriving hardness and elastic modulus. In the early 1980s followed
the contributions of Newey et al. [11], and Pethica et al. [12]. In the
1990s renements to the instrumentation and methods for
extracting mechanical properties from the test enabled signicant
progress towards establishing nanoindentation as an important
tool [13,14]. Since that time, vigorous research on the further
development of the technique and its use in a range of materials
science research has been performed. This is highlighted by several
special focus issues of journals centered on instrumented
indentation testing. The most notable being the Journal of
Materials Research series which started in 1999 [15] and continued
in 2004 [16] and 2009 [17]. A special issue of Philosophical
Magazine focused on instrumented indentation testing also
appeared in 2006, resulting from the Engineering Conferences
International (ECI) conference in Crete in 2005 [18].
In addition to the seminal works cited above, there exists a
variety of excellent review articles which form the basis for
developing an understanding of the principles of the technique,
and outline the current state of understanding. These include those
presented by VanLandingham [19], Oliver and Pharr [20], Schuh
[21], Chudoba [22] and Golovin [2325]. The analysis of the
resulting data from the instrumented indentation test is underpinned by a fundamental continuum mechanics treatment of
surfaces, i.e., contact mechanics or surface mechanics. As such,
there are a variety of texts which address the underlying
continuum theory including those of Johnson [26], Fischer-Cripps
[27] and Ling et al. [28]. Texts which include particular emphasis
on instrumented indentation testing include those by Bulychev
and Alekhlin [29], Herrmann et al. [30] and Golovin [31].
Instrumented indentation testing (IIT) has emerged as an

important method for the evaluation of a materials mechanical
response to applied loading. The technique is based on the
continuous recording of applied force and resulting depth of
penetration of an indenter throughout the whole loading and
unloading cycle, when applied force is controlled. Displacement
control is also possible. The technique allows for the determination
of the traditional values of hardness without the need to measure the
residual size of an indentation produced by an applied force. Initially
used for the evaluation of hardness and elastic modulus of small
material volumes and thin lms, emerging uses are for the evaluation
of a broad range of material mechanical behavior including work of
elastic and plastic deformation, fracture, time-dependent behavior,
residual stresses, and dislocation behavior and the onset of
plastic deformation. Techniques are currently being developed to
enable the determination of material constitutive behavior (i.e.,
stressstrain behavior) as well. Whereas it was rst referred to as
ultra-microhardness testing or nanoindentation testing because of
the force and length scales involved, today, instrumented indentation testing is meant to encompass a much broader range of forces
(up to 30 kN) and resulting indentation depths. In the present work
we will focus on the lower end of the applicable range of
instrumented indentation testing, i.e., nanoindentation.
1.1. Brief history of development
The origins of the technique can be thought to have rst
occurred at the end of the nineteenth century when Martens
presented a device which allowed for the measurement of test
force and indentation depth [1]. In the second half of the twentieth
* Corresponding author.
E-mail address: lucca@ceat.okstate.edu (D.A. Lucca).
0007-8506/$ see front matter 2010 CIRP.
doi:10.1016/j.cirp.2010.05.009
804
D.A. Lucca et al. / CIRP Annals - Manufacturing Technology 59 (2010) 803819
1.2. Standards and international comparisons

The rst standard developed to address a test method for
measuring Universal Hardness (now Martens Hardness) was DIN
50359-1 to -3 in 19971998 [32]. It dened the test method, as
well as the methods for the verication and calibration of hardness
testing machines. It was this German standard that provided the
basis for the development of the international standard ISO 145771 to -3 on instrumented indentation testing which was published
in 2002. ISO 14577 Metallic materialsInstrumented indentation
test for hardness and materials parameters contains the following
parts [33]:
ISO 14577-1 Part 1: Test method.
ISO 14577-2 Part 2: Verication and calibration of testing
machines.
ISO 14577-3 Part 3: Calibration of reference blocks.
ISO 14577-1 denes three application ranges of instrumented
indentation testing:
Nano range: hmax 200 nm.
Micro range: hmax > 200 nm and Fmax < 2 N.
Macro range: 2 N Fmax 30 kN.
where hmax is the maximum indentation depth and Fmax is the
maximum test force.
The standard does not specically address the indentation of
coatings and thin lms, and as a result of the European project
INDICOAT [34] led by the National Physical Laboratory (NPL) in the
UK, ISO 14577-4 Part 4: Test method for metallic and non-metallic
coatings was published [35]. Also contributing to the development
of the ISO 14577 standard was the work of VAMAS (Versailles
Project on Advanced Materials and Standards) with the European
pre-standard ENV WI 152 Determination of hardness and Youngs
modulus by instrumented indentation testing [36]. It described a
method for measuring hardness and elastic modulus of ceramic
coatings by instrumented indentation testing. In 2007, the
standard ASTM E 2546-07 Standard Practice for Instrumented
Indentation Testing [37] was introduced in the United States.
Similar to ISO 14577-1, the standard covers test ranges from the
nano to macro range. It also contains annexes which include: A1.
Instrument Verication, A2. Standard Reference Blocks and A3.
Indenter Requirements. An Interlaboratory Study [38] was
conducted which allowed for the establishment of precision
statements for ASTM E 2546-07 which are included in an
additional appendix to the standard. As a further extension to
the ISO standards, recently ISO/TR 29381:2008 Metallic materials
measurement of mechanical properties by an indentation test
Indentation tensile properties was published [39]. This document
establishes methods for the evaluation of tensile properties of
metallic materials (i.e., true stressstrain curves) using instrumented indentation testing, and is further discussed in Section 5.
Recently, based on a proposal from NPL, ISO TC164/SC3 is
preparing a new work item on the nanoindentation test for
viscoelastic materials [40].
In parallel to the development of standards there have been a
variety of international comparisons which have contributed to
standard development. The rst international comparison on
nanoindentation sponsored by the Scientic Technical Committee
on Surfaces (STC S) of the International Academy for Production
Engineering (CIRP) was carried out over the period 19931997.
Another comparison was conducted within the framework of
VAMAS and organized by the Federal Ofce for Materials Testing
(BAM) in Germany and NIST in the USA [41]. At the time of these
comparisons international standards for test and calibration
procedures did not exist, and participants could only rely on
procedures which they had developed or which were provided by
instrument manufacturers. The EU project INDICOAT on coatings
mentioned above was also completed before an international
standard existed. With the emergence of ISO 14577, and
improvements in the indentation instruments a second CIRP

sponsored comparison was held from 20052009 with the
objective to determine how well ISO 14577 could be realized
[42]. Details of the two CIRP sponsored comparisons are further
described in Section 4.
1.3. Motivation
This current paper evolved from the most recent collaborative
activity on nanoindentation sponsored by the STC S of the CIRP.
Since a variety of excellent reviews on nanoindentation already
exist, this contribution is not meant to be a complete review of the
eld of nanoindentation or more broadly, instrumented indentation testing, nor has any attempt been made to be all inclusive.
Instead the focus is on presenting one view of the current state of
the method, the standards which have emerged, methods for
verication and a few examples of emerging applications. As the
method moves from the research laboratory towards its development as a useful tool for quality control purposes there will be a
continued need to further develop verication and calibration
methods, and uncertainty analyses.
In the section to follow we present the measurement method,
the instruments currently in use and the procedures for the
analysis of the resulting data. This is followed by a section on the
methods so far developed for verication and calibration including
a discussion on uncertainty of parameters. We then summarize the
results of the most recent CIRP sponsored comparison on
nanoindentation and compare the results to those obtained in
the rst such comparison. Finally, a brief look at some of the
emerging uses of the technique including its use for the
determination of the constitutive behavior of materials, and in
investigations of biomaterials and time-dependent behavior.
2. Measurement method and data analysis
The measurement method and data analysis of the instrumented indentation test is given in full detail in ISO 14577-1, Part 1
[33]. The method and data analysis were developed for metallic
materials however they are also suitable for many glasses,
ceramics and semiconductors. The method and data analysis
however are not typically well suited for the evaluation of rubbers
and other highly elastic materials. This section summarizes the
important aspects of the ISO document and provides additional
material that has been published since the standard was adopted.
2.1. Method
During an instrumented indentation test the applied test force
and the indentation depth of the indenter are continuously
measured. Typical indenter materials include diamond, tungsten
carbide, and sapphire. Commonly used indenter geometries
include: pyramidal with square base (Vickers), pyramidal with
triangular base (Berkovich and cube corner) and spherical. Fig. 1
shows the geometry of the Vickers and Berkovich indenters. The
Vickers indenter has an angle of 1368 between opposing faces of
the pyramid. The Berkovich indenter has an equilateral triangle as
the base and an angle of 65.038 between the axis of the pyramid
and the three faces. The cube corner indenter is similar to the
Fig. 1. Geometry of Vickers indenter, left, and Berkovich indenter, right.
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Fig. 2. Berkovich indenter measured by a metrological atomic force microscope.
Berkovich indenter however the angle between the axis of the

pyramid and the three faces is 35.268. Fig. 2 shows an image of a
Berkovich indenter obtained by a metrological atomic force
microscope.
Either the force or the displacement of the indenter is controlled
by the indentation instrument during the testing cycle. Fig. 3
shows an example of a testing cycle for a force-controlled
instrument. The testing cycle is composed of a linear loading to
the maximum force in 30 s, a 30 s hold at the maximum force to
allow time-dependent plasticity or creep effects to diminish, a 10 s
unloading to 10% of the maximum force, a 60 s hold at this force to
measure the thermal drift of the instrument followed by a 2 s nal
unloading. The times given here are reasonable for many materials
however the time of the hold period at the maximum load should
be chosen such that the unloading curve is not signicantly
inuenced by the creep of the test piece. Chudoba and Richter have
suggested hold times for some common materials ranging from
fused silica with a hold time of 8 s to aluminum with a hold time of
187 s [43]. To minimize the effects of creep and thermal drift on the
unloading curve the unloading rate is typically higher than the
loading rate.
Fig. 4 shows the results of an indentation test using the test
cycle shown in Fig. 3. The test force is plotted as a function of the
indentation depth. The curve (a) shows the application of the test
force, the hold at maximum force (Fmax) is designated by (b), the
rst part of the unloading is shown by curve (c), the hold at 10% of
the maximum force is shown by (d) and the nal unloading occurs
during (e). The line (f) is the tangent line to the unloading curve at
the maximum test force and hr denotes where this line intersects
the depth axis. The slope of the line (f) and the value hr are used in
the analysis of the data as described in Section 2.3. The maximum
depth during the indentation is given by hmax and the depth of the
permanent deformation of the test piece is given by hp.
The indentation depths during and after an indentation test are
shown schematically in Fig. 5. The total depth of indentation while
the test force is applied is given by h, Fig. 5(a). The indenter and test
piece are in contact with one another from the indenter tip to a
depth hc, the contact depth. The difference between the total depth,
h, and the contact depth, hc, is given by hs. After the removal of the
Fig. 3. Typical test force vs. test time cycle for indentation.
Fig. 4. Test force vs. indentation depth plot. See text for explanation of annotations.
test force the depth of the permanent deformation in the test piece
is given by hp, Fig. 5(b). The accurate determination of these depths
requires the accurate assessment of the zero point of the depth. The
ISO standard 14577 [33] species that the uncertainty in the zero
point determination should be less than 1% of the maximum
indentation depth for the macro and micro range. For the nano
range the uncertainty may be greater than 1%, however it should be
estimated and recorded.
The ISO standard further stipulates that the test piece should be
free of extraneous matter and should be aligned such that the
surface is perpendicular to the test force direction. The surface
should be prepared in such a way that alterations to the near
surface hardness are minimal. The surface roughness Ra of the test
piece should be less than 5% of the maximum indentation depth for
the macro and micro range. In the nano range this may not always
be possible. To exclude the inuence of the test piece support on
the measurement of hardness and elastic modulus the thickness of
the test piece should be greater than 10 times the maximum
indentation depth or 3 times the maximum indentation diameter,
whichever is greater.
2.2. Instruments
There have been a variety of instruments developed for
performing instrumented indentation; Table 1 shows a sample
of instruments that are currently commercially available. The
Fig. 5. Schematic drawing of indentation surface showing (a) indenter with applied
test force and (b) after removal of the test force. Indentation depth under applied
test force, h, depth of contact of the indenter with the test piece hc, depth below
surface not in contact with indenter hs and permanent indentation depth after
removal of test force hp, are denoted.
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Table 1
Sample of indentation instruments and the measurement systems employed.
Instrument
Force measurement
system
Displacement
measurement
system
Picodentor HM500 (Fischer)

Nano Indenter G300 (Agilent)
Nano Test (Micromaterials)
Triboindenter TI 950 (Hysitron)
Ultra Nano Hardness Tester (CSM)
IBIS (Fischer-Cripps)
UNAT (ASMEC)
Electromagnetic
Electromagnetic
Electromagnetic
Capacitive
Capacitive
Inductive
Inductive
Inductive
Capacitive
Capacitive
Capacitive
Capacitive
Inductive
Inductive
measurement systems used include electromagnetic, capacitive

and inductive systems for the measurement of the force, and
inductive and capacitive systems for the measurement of the
displacement of the indenter. Table 2 shows the capabilities of
these instruments in terms of the range and digital resolution of
the force and displacement systems. All values given are as
reported by the manufacturer. Whereas the noise level is a better
parameter for comparison than the digital resolution, it is
sometimes not provided by the manufacturer. Many instruments
come with multiple measurement heads which can increase the
range of the measurements. In addition to these commercial
systems, a variety of research laboratory-developed systems exist.
One such system developed at the PTB is a MEMS-based
nanoindenter which uses an electrostatic comb drive [44], shown
in Fig. 6. The indenter is a spherical ball of either 50 or 100 mm
diameter that is attached to a V-groove in the shaft of the
electrostatic comb drive.
Additions to basic indentation systems have been introduced to
extend their capability. Continuous Stiffness Measurement (CSM)
uses a small ac signal that is superimposed on the force loading/
unloading cycle to measure the contact stiffness throughout the
complete cycle. From the contact stiffness the indentation
modulus can be calculated throughout the cycle. For viscoelastic
test pieces continuous stiffness measurement can be used to
determine the storage modulus and the loss modulus, as described
in Section 5.2. Some of the important issues of using CSM for the
measurement of properties at small depths have recently been
discussed by Pharr et al. [45]. Another instrument that uses an
oscillating indenter is the NanoScan instrument which uses a
method similar to Ultrasonic Contact Impedance (UCI) to measure
a shift in the resonant frequency as a function of indentation depth
[46]. Special heated stages and thermal isolation of the depth and
force systems have also been developed which enable indentation
measurements up to 750 8C. Experiments at high temperature
have provided insight into dislocation nucleation [47]. Systems
have been developed which enable the rapid application of the test
force thus resulting in a nano-impact test. Nano-impact testing has
been used to show a relationship between nano-impact and tool
wear life in the end milling of AISI 1040 steel with TiAlN or AlCrN
coated tools [48]. Indentation has also been combined with
Transmission Electron Microscopy (TEM) to investigate the initial
stages of plastic deformation [49,50]. In an investigation of the
indentation behavior of aluminum Minor et al. [49] showed the
Fig. 6. MEMS-based nanoindenter developed at the PTB [44]. (a) Schematic diagram
of the nanoindenter showing the electrostatic comb drive and (b) close-up of the
indenter holder where the indenter is a spherical ball of 100 mm diameter.
initial dislocation nucleation and subsequent dislocation multiplication. Fig. 7 shows frames from a video of the indentation
process where the indenter is at the bottom of the images and the
aluminum is above. The time from the start of the experiment is
shown in seconds in the upper right corner of the images. The rst
frame (a) shows that the aluminum is dislocation free in the area to
be indented. In (b) and (c), contact has been made however the
deformation is still elastic. Between frames (c) and (d), dislocations
are nucleated. In (e) and (f), the multiplication of dislocations is
shown. Indentation instruments have been modied to include
Table 2
The range and digital resolution of the force and displacement systems as given by
the manufacturers.
Instrument
Fmax (N)
Force
resolution
(nN)
hmax
(mm)
Displacement
resolution
(nm)
Picodentor HM500
Nano Indenter G300
Nano Test
Triboindenter TI 950
Ultra Nano Hardness Tester
IBIS Model B
UNAT
0.5
0.5
0.5
10a
0.1
0.05, 0.5
2
100
50
30
1
1
70
100
150
500
50
0.04
0.01
0.001
0.02
0.001
0.003
0.01
With optional head.
100
2, 20
150
Fig. 7. Still frames of video from TEM observation of indentation in aluminum [49].
Indenter is in the bottom portion of the frames and aluminum is above. Time in
seconds is shown in the upper right of each frame. Plastic deformation is initiated
sometime in between frames (c) and (d).
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depth. The intercept of the depth axis by the tangent line to the
unloading curve determines the depth hr, as shown in Fig. 4. The
contact depth, hc, is calculated from:
hc hmax ehmax hr
(1)
where e is 0.75 for a Berkovich or Vickers indenter. With knowledge

of the contact depth and the area function of the indenter the
contact area can be calculated. The indentation hardness HIT, is
given by:
HIT
F max
Ap hc
(2)
where Fmax is the maximum test force and Ap(hc) is the projected
area of contact of the indenter evaluated at a depth of hc. The
indentation modulus EIT can be calculated from the following two
equations:
EIT
Er
Fig. 8. Scratch test results for amorphous carbon lms (a-C:H) containing silicon.
The micrographs are for a 614 nm thick lm (top) and a 366 nm thick lm (bottom).
Large uctuations in the penetration depth are associated with spalling of the lm
[51].
1 ns 2
1=Er 1 ni 2 =Ei
p
p
p
2C Ap hc
(3)
(4)
where ns is Poissons ratio of the test piece; ni is Poissons ratio of

the indenter; Er is the reduced modulus of indentation contact; Ei is
the elastic modulus of the indenter; C is the compliance of contact,
i.e., dh/dF of the test force removal curve evaluated at the
maximum test force; Ap(hc) is the projected contact area.
Since the development of the above expressions for the
evaluation of indentation hardness and modulus from indentation
data there have been modications to correct some minor
problems in the original analysis. The original solution to the
problem assumed a constant value of e equal to 0.75 for a Berkovich
or Vickers indenter. More correctly e can be calculated from the
exponent m by [20]:

2G m=2m 1
m 1
(5)
e m 1 p
pG 1=2m 1
another axis of motion and thus enable the instrument to perform

scratch tests. Scratch testing has been used for a variety of
applications including the determination of the friction between
the indenter and the test piece, the determination of the fracture
toughness of lms [52], and the determination of the adhesion of
the lm to the substrate [51,53]. Fig. 8 shows the results of a
scratch test performed on amorphous carbon lms (a-C:H) which
contain silicon [51]. The micrographs are for two different lm
thicknesses: 614 nm for the top micrograph and 366 nm for the
bottom. The experiment was performed with a 0.5 mm radius
indenter which traversed 250 mm. The normal force on the
indenter was increased from 0.05 mN to 100 mN at a constant rate
of 1 mN/s. Spalling of the lm was accompanied by large
uctuations in the penetration depth. As opposed to macro scratch
testing with a constant load per unit scratch distance there was no
clear dependence of the critical load on the loading rate or
scratching speed. Although the scratch test can provide comparative information, there are signicant difculties in obtaining
quantitative adhesion data from the test [53].
where G is the gamma function. For many materials m is in the

range of 1.21.6 which means that e varies from 0.79 to 0.74. The
average value is about 0.76 which is close to the assumed constant
value of 0.75. Another modication to the analysis corrects for the
radial displacement of the test piece in contact with the indenter.
Using the original analysis of Sneddon [54] the predicted radial
displacement of the test piece would be inside of the boundary of
the indenter, which of course is physically impossible. Hay et al.
[55] propose a few approximations for correcting this problem.
One solution is the calculation of a correction factor g given by:
2.3. Analysis of data
g 1
The basic analysis of instrumented indentation data has its

foundation in the elastic contact theory of Hertz. More recently the
works of Oliver and Pharr [14] and Field and Swain [13] have been
developed. For the determination of both the elastic modulus and
the hardness, the area of contact between the indenter and the test
piece is required. The area of contact can be determined from
knowledge of the indenter geometry and the contact depth, hc
through the area function of the indenter. The area function gives
the area of the indenter as a function of the distance from the tip of
the indenter. In the Field and Swain method for indentation with a
spherical indenter, two points on the unloading curve are used to
determine the contact depth whereas in the Oliver and Pharr
method the slope of the unloading curve ((c) in Fig. 4) is used to
determine the contact depth in the following manner. The upper
80% of the unloading portion of the force vs. depth curve is t to the
equation F = K(hhp)m where F is the force, h is the depth, hp is the
plastic depth, and K and m are constants. This expression is then
differentiated with respect to the depth to obtain the slope of the
unloading curve which is evaluated at the point of maximum
where f is the half-included angle of the indenter. For a Berkovich

indenter the equivalent half-included angle is 70.328. This results
in a correction of approximately 1.04 for aluminum and a
correction of approximately 1.07 for fused silica. The correction
factor is then used in Eq. (4) such that
p
p
p
Er
(7)
2g C Ap hc
1 2ns
41 ns tan f
(6)
Chudoba and Jennett arrived at a similar result by considering a

correction factor for the area [56]. Without the correction the
reduced elastic modulus is overestimated by approximately 510%
depending on the indenter geometry and Poissons ratio of the test
piece.
In addition to the indentation modulus and indentation
hardness, other properties can be derived from the instrumented
indentation test. Some of those given by ISO 14577-1 [33] are
shown in Table 3. Martens hardness, HM, differs from the
indentation hardness in two ways. Firstly it is calculated using
the indentation depth, h not the contact depth, hc. Because the
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Table 3
Properties derived from the instrumented indentation test.
Elastic or elasticplastic properties
Plastic properties
Indentation modulus, EIT

Martens hardness, HM
Martens hardness, from the slope
of the increasing force curve, HMS
Indentation relaxation, RIT
Elastic deformation work, Welast
Elastic part of indentation work, hIT
Indentation Hardness, HIT

Indentation Creep, CIT
Plastic deformation work, Wplast
Yield strength, sy
indentation depth is used, Martens hardness includes the elastic

and plastic response of the test piece whereas the indentation
hardness, HIT, represents the plastic response. Secondly the area
used for the calculation of Martens hardness is the surface area of
the indenter, not the projected area. Martens hardness is most
often calculated at the maximum test force and depth and is given
by HM = Fmax/(As(hmax)). Martens hardness can also be calculated
from the slope of the increasing force curve. The curve is assumed
to be of the form h = mF1/2 where the constant m is determined by a
curve t of the increasing force curve between 50% of Fmax and 90%
of Fmax. Martens hardness is then calculated from HMS = 1/
(m2As(h)/h2). This calculation avoids the error associated with
the incorrect determination of the zero point however it can only
be used for larger depths where the inuence of tip rounding can
be neglected.
Indentation creep is the change in the depth that occurs at a
constant test force. For example in Fig. 4, (b) shows there is a small
increase in the depth at a constant load of 10 mN. Indentation
creep is calculated as CIT = (h2 h1)/h1 100 where h2 is the depth
after a certain hold period and h1 is the depth at the start of the hold
period. In tests where the depth is controlled there can be a change
in the force that occurs at a constant depth. This is referred to as
indentation relaxation and is calculated in a manner similar to the
indentation creep: RIT = (F2F1)/F1 100 where F2 is the force after
a certain hold period and F1 is the force at the start of the hold
period.
The total mechanical work of indentation can be determined by
computing the area under the force increasing portion of the test
force vs. indentation depth curve. The total work can be divided
into two components: elastic and plastic. The elastic work can be
determined by the area under the force decreasing portion of the F
vs. h curve, and the plastic work can be determined from the area
between the force increasing and force decreasing curve. The
elastic part of the indentation work is calculated as: hIT = Welast/
Wtotal 100 where Welast is the elastic work and Wtotal is the total
work. There have been some attempts to use work in the
calculation of hardness and elastic modulus [57,58] however
these methods are not yet in the ISO standard. The yield strength of
the test piece can also be determined as discussed in Section 5.1.
In addition to the above-mentioned properties obtained from
the instrumented indentation test, other behaviors have been
observed. For example, Fig. 9 shows a test force vs. indentation
depth curve for an indentation in 1 0 1 0 ZnO. At a test force of
approximately 160 mN there is a sudden increase in indentation
depth. This behavior, referred to as pop-in, has been observed for
a variety of materials including metals and semiconductors. The
behavior is most often attributed to the nucleation of dislocations
and the onset of plasticity [59,60] although in some cases it has
been attributed to the breakthrough of an oxide layer [61]. Fig. 10
shows another type of discontinuity in the test force vs.
indentation depth curve that can occur during the unloading of
the test piece. Here the unloading curve of (1 1 1)Si shows popout and an elbow that are associated with phase transformations of silicon [63]. Similar behavior has been observed in other
materials including Ge, diamond and ZrO2 [23].
In addition to phenomena observed in the test force vs.
indentation depth curve, hardness results have also shown
interesting phenomena. Fig. 11 shows hardness as a function of
contact depth for the indentation of two different surface
Fig. 9. Test force vs. indentation depth curve for the indentation of 1 0 1 0 ZnO
showing pop-in at a force of approx. 160 mN. After [62].
orientations of ZnO, (0 0 0 1) and 1 0 1 0. In both cases the

indentation hardness is found to increase as the contact depth
decreases. This indentation size effect has been observed in many
different materials, and has most often been attributed to a
physical mechanism as described by strain gradient plasticity [64].
The method for determination of the mechanical properties of
coatings is given in detail in Part 4 of ISO 14577 [35]. An outline of
the method follows here. The method is limited to the indentation
of a single coating on a substrate. For the evaluation of the plastic
properties of the coating, indentation with a pointed indenter is
recommended, and for the evaluation of the elastic properties of
the coating, indentation with a spherical indenter is recommended. A spherical indenter with a larger radius has the
advantage of enabling fully elastic deformation at reasonably
large depths, however has the disadvantage of surface effects (e.g.,
roughness) creating larger uncertainties in the measurement. To
extract the coating properties from the measured results,
indentations over a range of depths are performed. Indentations
Fig. 10. Test force vs. indentation depth for indentations in (1 1 1)Si. The observed
pop-out and elbow in the unloading curve are attributed to phase
transformations of the silicon [63].
809
Fig. 13. Indentation hardness vs. normalized contact depth of DLC coatings on
hardened tool steel. The thicknesses of the coatings were ^ 2510 nm, &1470 nm
and ~ 460 nm [35].
Fig. 11. Indentation hardness vs. contact depth for two different surfaces of ZnO.
The hardness is found to exhibit the size effect, i.e., the hardness increases as the
indentation depth decreases. After [62].
are performed at a minimum of three different, and preferably ve

or more, maximum forces. The measured indentation modulus or
hardness is plotted as a function of the indentation contact depth,
hc, or radius of contact, a, normalized by the lm thickness, tc.
Fig. 12 shows the plane strain indentation modulus vs. the
normalized radius of contact for a Diamond-Like Carbon (DLC)
coating on a hardened tool steel substrate. The plane strain
indentation modulus is EIT/(1 n2s ). The dashed line 1 shows the
plane strain indentation modulus of the steel. The plane strain
indentation modulus of the coating is obtained by tting a line to
the shallow indentations and extrapolating to zero normalized
radius. In this case the plane strain indentation modulus of the DLC
coating is found to be 170 GPa, dashed line 2. In general, for soft/
ductile coatings the range a/tc < 1.5 should be used for the linear
t, and for hard/brittle coatings the range a/tc < 2 should be used.
As seen in Fig. 12 however, judgment must be used to determine
the appropriate range for a given test piece.
The determination of the hardness of a soft coating on a hard
substrate can be obtained in a manner similar to that for the
determination of elastic modulus. In this case however a pointed
indenter is used and the contact depth normalized by the coating
thickness is plotted on the abscissa. The maximum depth of
penetration must be shallow enough such that the deformation of
the substrate is only elastic. The linear region of HIT depends on the
ratio of the substrate hardness to coating hardness. For a hardness
ratio of 2.5 the limit of hc/tc < 1 and for a hardness ratio of 8 the
limit of hc/tc can reach 5.
For the case of a hard coating on a soft substrate, a pointed
indenter with a small included angle should be used to cause
yielding in the coating rather than the substrate. The range of
indentation depths should be selected such that the indentation

hardness is a maximum in this range, usually 0 < hc/tc < 0.5. If a
plateau in hardness values is observed in this range, this value is
taken as the hardness of the coating. For example, in Fig. 13 the DLC
coatings on a steel substrate with a coating thickness of 2510 nm
(^) and 1470 nm (&) exhibit a plateau in hardness at approximately 17 GPa. If no plateau in hardness values is observed and
only a maximum is observed, indentations should be made on
thicker coatings. If the same maximum hardness is observed on the
thicker coatings as well, this is a strong indicator that this is the
hardness of the coating. In Fig. 13 the hardness of the 460 nm thick
coating (~) cannot be resolved as the data exhibit a maximum of
approximately 15.5 GPa and the indentations on thicker lms
produce a higher hardness.
3. Verication and calibration
Verication and calibration of indentation instruments is
presented in detail in Part 2 of ISO 14577 [33]. The standard
covers the macro, micro and nano ranges; in this section the nano
range will receive more emphasis. Important points to consider
when calibrating in the macro and micro range are given in [65].
This section will summarize the standard and provide additional
information. Also, a discussion of the assessment of uncertainty of
the results obtained by instrumented indentation is included.
3.1. Verication and calibration of indentation instruments
Verication can be divided into two types: direct verication for
checking the main functions of the indentation instrument, and
indirect verication for determining the repeatability and for
periodic checking of the instrument. Table 4 shows the main
calibration quantities and the measurement methods typically used
to obtain these quantities. These items are discussed in detail below.
Direct verication involves the verication or calibration of the
quantities given in Table 4. The verication of the indenter
geometry should be performed by a qualied calibration laboratory and a calibration certicate for the indenter should be
Table 4
Calibration and verication quantities and typical measurement methods.
Calibration quantity
Measurement methods
Indenter geometry
Test force
Optical microscopy, AFM

Electronic balance, deadweights, calibrated
bendable beam, nanoforce sensor
Laser interferometry, capacitance sensor, LDVT
Indentations in reference materials
Metrological AFM, indentations in reference
materials
Clock with 0.1 s uncertainty
Indentation depth
Machine compliance
Indenter area function
Fig. 12. Plane strain indentation modulus vs. normalized contact radius of
Diamond-Like Carbon (DLC) coating on hardened tool steel [35].
Testing cycle
810
provided. The geometry of the indenter should be veried so that it

conforms to the ISO 14577-2. For example, for a Vickers indenter
the angle between the opposing faces should be 136 0.38. Other
values include the allowable rounding of the indenter tip and the
maximum permissible angle between the diamond pyramid axis and
the axis of the indenter holder. Calibration of the test force should be
performed by a traceable method. Some of the methods for measuring
the test force are given in Table 4. For the nano range, an electrostatic
balance has been developed as a standard at NIST for forces between
108 and 104 N [66]. As shown in Fig. 14, the instrument is housed in
a vacuum enclosure which is approximately 1 m in diameter and uses
a coaxial cylindrical capacitor arrangement for the generation of
force. A secondary artifact calibrated by the electrostatic balance
could be used to calibrate the test force of indentation instruments.
For example a piezoresistive cantilever could be used as a secondary
artifact for the calibration of force [66]. The electrostatic balance has
also been used to calibrate deadweights in the range of 0.5 mg to
500 mg (approximately 5 mN to 5 mN) which could be used for the
calibration of the indentation force in the nano range. Other devices
based on silicon springs have also been developed [67,68]. An
advantage of these devices is their relative ease of fabrication as they
are fabricated using standard photolithography and MEMS techniques. Fig. 15 shows the top view of a passive silicon spring where the
force to be measured would be applied to the center of the spring. The
spring is linear with a spring constant of approximately 19 mN/mm in
this case [67]. In another design, a capacitance gage is integrated into
the device [68]. The capacitance between a xed plate and a moveable
plate that rests on the springs is measured by a high-resolution
capacitance bridge. This system has been calibrated over the range 5
5000 mN. Fig. 16 shows a close-up view of a multi-functional
nanoforce actuator [69]. This actuator uses an electrostatic comb
drive to generate forces up to approximately 1 mN for an applied
voltage of 50 V. The resolution of the actuator is approximately 1 nN.
For the calibration of the indentation depth, a measuring system
based on laser interferometry, a capacitance sensor or an inductive
Fig. 15. Top view of silicon spring based device for the calibration of test force and
indentation depth [67].
sensor is most commonly used. The measuring system must be

graduated such that the resolution meets the requirements given in
Table 5. The table also shows the maximum permissible error of the
measurement for the three indentation ranges. The indentation depth
should be calibrated at a minimum of 16 points evenly distributed
throughout the range of the indentation instrument. The measurements should be repeated at least three times. Verication of the
testing cycle should be performed with a clock with an uncertainty of
0.1 s. The times of the application of test force, hold period at
maximum test force and removal of test force should all be veried.
For indentations with a depth less than 6 mm the area function
of the indenter must be measured. One means of measuring the
area function of the indenter is with a metrological AFM. An image
obtained by such a measurement is shown in Fig. 2. The area
function determined by this measurement was found to have a
relative uncertainty of 8% at 200 nm [70]. Another common
approach is to determine the area function of the indenter and the
machine compliance simultaneously using an iterative procedure
[14,35]. In this procedure, calibrated reference materials with two
different elastic moduli are required. The means of establishing a
certied reference material are given in ISO 14577, Part 3 and in
the report of the EU project DESIRED [33,71]. For best results the
modulus values of the two reference materials should be
signicantly different from each other. Typical materials include
tungsten, E 410 GPa, fused silica, E 72 GPa and aluminum,
Fig. 16. Nanoforce actuator with multifold springs [69]. Central shaft of actuator is
on the right of the image.
Table 5
Resolution and maximum permissible error of the displacement measuring system
[33].
Fig. 14. NIST electrostatic force balance: (a) complete system including vacuum
enclosure, (b and c) close-up of balance [66].
Range of
application
Resolution of the
displacement measuring
device (nm)
Maximum permissible
error
Macro
Micro
Nano
100
10
1
1% of h
1% of h
2 nm, preferably 1% of h
E 70 GPa. To begin the procedure a series of indentations in the

reference material with the lower hardness or higher elastic
modulus is performed. These indentations are performed at two
or more different depths. The data are then used to obtain an initial
estimate of the machine compliance. For this rst iteration the area
function of the indenter is assumed to be that of an ideal indenter. To
obtain the machine compliance, a plot of Ct vs. 1/(Ap(hc))0.5 is made
and the y-intercept of a line through the data gives the rst estimate
of the machine compliance. This can be seen from the following:
p
p
1
p
Ct Cf
(8)
2Er Ap hc
where Ct is the total measured compliance and Cf is the machine
compliance. The machine compliance is given by a single constant
value however in reality the compliance may be a function of the
force. A large elastic modulus or deep indentations will make the
second term in Eq. (8) small, thus providing a better estimate of the
machine compliance. Indentations in the second reference
material are performed at multiple depths distributed over the
range of depths for which the indenter will be used. The area is
then calculated by:
Ap hc
p 1
1
4 Er 2 C t C f 2
(9)
using the value of Cf estimated from Eq. (8). An area function,

typically of polynomial form, is then obtained by tting the values
of area obtained from Eq. (9). Originally an area function of the
following form was suggested [14]:
2
Ap hc C 0 hc C 1 hc C 2 hc
1=2
C 3 hc
1=4
C 8 hc
1=128
(10)
More recently however, truncated forms of this equation have

been found to describe the area function with fewer terms and
higher accuracy [34,72]. Because the area function has an inuence
on the machine compliance value, the entire analysis is repeated
until convergence is achieved. An alternative method for the
determination of the machine compliance consists of xing the
indenter to the measuring table and applying a test force. The
change in indicated indentation depth can then be used to obtain
the machine compliance [71].
Indirect verication to determine the repeatability of the
indentation instrument and to periodically check the instrument is
performed using calibrated reference materials. The reference
materials can be calibrated for hardness or indentation modulus.
Two reference materials should be chosen such that their reference
values fall in two different measurement ranges as dened in
Table 6. Indentations should be performed at a minimum of two
test forces and should be at the forces that are most frequently
used. For indentations greater than 6 mm deep, at least ve repeat
indentations in each reference material at each test force should be
performed. For indentations less than 6 mm, at least ten repeat
indentations should be made. The mean and experimental
standard deviation of the measured hardness or indentation
modulus for each reference material and each test force should be
computed. Further, the coefcient of variation, CV, which is a
measure of the relative scatter of the data should be computed as:
CV
sq
q
(11)
where s(q) is the experimental standard deviation and q is

the average value. The coefcient of variation indicating the
repeatability of the indentation instrument is considered satisfacTable 6
Range of hardness and indentation modulus values for indirect verication [33].
Range
Hardness, HM or HIT (MPa)
Indentation modulus, EIT (GPa)
Low
Medium
High
2500
25007000
>7000
50100
100450
811
Table 7
Maximum limits of the coefcient of variation for satisfactory repeatability of
indentation instruments [33].
Material
parameter
Micro range
0.2 mm h 1 mm
Micro range h > 1 mm
Macro
range
HM, HIT
EITa
5%
5%
2%
5%
2%
5%
For nearly perfectly plastic materials these limits may not be achievable.
tory if it meets the requirements given in Table 7. It should be

noted that in the current ISO standard there are no limits given for
the nano range.
The ISO standard provides guidelines for the interval between
verications [33]. A full direct verication of the indentation
instrument should be performed when the instrument is new. A
limited, direct verication of the test force, indentation depth, and
testing cycle should be performed when (1) the instrument is
installed or moved, (2) an indirect verication has given
unsatisfactory results or (3) the last verication was over three
years prior. After a full or limited direct verication, an indirect
verication should be performed. The maximum interval between
indirect verications is one year. In addition it is suggested that
routine checks are carried out before and after a series of tests or
periodically (e.g., daily) within a test series. For routine checking,
indentations at two different test forces should be performed on a
calibrated reference material. Three to ve repeat indentations
should be made at each test force. The results of these tests should
be recorded and plotted as a function of time to display any
changes in the instrument with time.
3.2. Uncertainty of the measurements
Guidelines for the estimation of uncertainty in the measurement
of hardness obtained by hardness testing machines have been
established [73]. For instrumented indentation testing however,
there are currently no such guidelines. However, two methods for
the estimation of uncertainty in instrumented indentation testing,
based on the general principles presented in the Guide to the
Expression of Uncertainty in Measurement (GUM) [74], have been
developed. These methods have been mostly applied to the
evaluation of the uncertainty in hardness and indentation modulus,
however they could also be applied to other properties listed in
Table 3 with appropriate modication. The rst method evaluates
the uncertainty based on indentations in a reference material. The
expanded uncertainty Ux for a material parameter x such as
indentation hardness or indentation modulus can be determined
from [75]:
p
U x k uRMx 2 uRMx 2 ux 2 umsx 2 ubx 2
(12)
where k: coverage factor of expanded uncertainty (k = 2); uRMx:

standard uncertainty of the material parameter x for which the
reference material was calibrated; uPMx: standard uncertainty of
the indentation instrument for material parameter x measured on
reference material; ux : standard uncertainty of measurement
parameter x on test material; umsx: standard uncertainty due to the
resolution of the indentation instrument; ubx: standard uncertainty of the correction b, if used.
The coverage factor k = 2 provides an interval having a level of
condence of approximately 95% if certain conditions are met [74].
The standard uncertainty of the material parameter x for the
reference material, uRMx, should be provided by the supplier of the
reference material. The standard uncertainty of the indentation
instrument for material parameter x on the reference material, uPMx,
can be determined by repeat indentations on the reference material.
The standard uncertainty is equivalent to the experimental standard
deviation of the mean and can then be obtained from [74]:
uPMx
r
s2 xk
(13)
812
where s(xk) is the experimental standard deviation of n repeated

indentations at a given test force. The standard uncertainty of
measurement parameter x on the test material, ux , is obtained in
the same way, i.e., by repeat indentations on the test material at a
given load and by the calculation of ux from the experimental
standard deviation using Eq. (13). The standard uncertainty due to
the resolution of the indentation instrument, umsx, is usually
negligibly small. The correction b refers to an offset that is applied
to the measurement results to account for systematic errors. There
is an uncertainty associated with this correction factor and it must
be included in the expanded uncertainty.
The second method for the determination of the uncertainty
combines the uncertainties from individual sources. The uncertainties of the individual sources are combined to form the
combined standard uncertainty (uc(y)) of measured value y by
using the partial derivatives as follows [74]:
uc 2 y

N
X
@f 2
@xi
i1
u2 xi
(14)
where the measured value y is a function of input variables xi such

that Y = f(X1, X2, . . ., XN). The lowercase values y and xi represent
estimates of the values Y and Xi. The value u(xi) represents the
uncertainty in the input xi. As an example consider indentation
hardness given by HIT = Fmax/Ap(hc). The combined standard
uncertainty is given by:
uc 2 HIT
1
Ap
u2 F max
HIT 2
Ap 2
u2 Ap
(15)
where Ap(hc) has been shortened to Ap for simplicity. Note that the
uncertainty terms u(Fmax) and u(Ap) should include all factors
which inuence the measured force and determination of the area
function. Hsu et al. performed this type of analysis for an
indentation instrument that operates in the nano range [76].
They found that the relative standard uncertainty of indentation
hardness was 6.3% and indentation modulus was 6.8% for
indentations with a depth of 100 nm or greater. In the micro
and macro range, Ullner analyzed the sources of uncertainty in the
instrumented indentation test for different materials [30,65]. The
material properties chosen corresponded roughly to those of iron,
aluminum, tungsten carbide and glass. Table 8 gives a summary of
the results obtained. The combined uncertainties for the macro
range were found to be less than those obtained for the micro
range. The Martens hardness determined from the slope of the
loading curve produced the highest relative uncertainty. Ullner
found that the machine compliance contributed signicantly to the
uncertainty in HMs [65]. He also found that the uncertainty in the
zero point determination could have a large inuence on the
combined uncertainty.
4. CIRP international comparison on nanoindentation
4.1. Introduction
By about 1990, nanoindentation was emerging as a useful
method for the determination of the micro or ultra-microhardness
of bulk materials and thin lms. Commercialized instrumentation
Table 8
Relative combined uncertainty of indentation properties for the micro and macro
range. After [65].
Property
Martens hardness, HM
Martens hardness from slope
of loading curve, HMs
Indentation hardness, HIT
Indentation modulus, EIT
Relative combined uncertainty (%)

Micro range, 1 N
Macro range,
100 N
67
820
34
517
68
68
35
46
was available having been developed at three or four research

centers worldwide. Very little information was available however,
on the achievable repeatability of measurements obtained with a
given instrument, or on the reproducibility or agreement between
measurements made with different instruments. It was therefore
decided in 1993 that the rst CIRP sponsored international
comparison of ultra-microhardness and elasticity measurements
would be conducted with the objective being to quantify the
repeatability and reproducibility which could be achieved with the
technique when measuring hardness and elastic modulus for a
series of bulk materials and coatings. Seven participants were
involved and measurements were made of the indentation
hardness and elastic modulus for a range of thin layers and bulk
materials. Specimens included steel, glass, single crystal silicon,
polymer and several thin lms prepared on soft and hard
substrates. Since there were no international standards on which
to rely, measuring and calibration procedures were carried out
according to the instructions of the manufacturers of the
instruments. A simple protocol was used and the test force ranged
principally from 5 mN to 100 mN with a few of the softer materials
examined down to 1 mN. For the measurement results of the
indentation hardness of steel, glass and single crystal silicon, the
coefcient of variation indicating repeatability was found to range
from 0.06 to 0.55, while the coefcient of variation indicating
reproducibility ranged from 0.23 to 0.59. Further details of the
intercomparison can be found elsewhere [77,78].
In light of the emergence of ISO 14577 in October 2002, it was
decided that a second comparison would be undertaken. The
objective of this comparison was to determine how well the ISO
standards (ISO 14577) could be realized. The PhysikalischTechnische Bundesanstalt (PTB) and Oklahoma State University
(OSU) agreed to be the pilot participants for this work. The exercise
involved twelve participants, listed in Table 9, throughout Europe,
Asia and the USA. The nanoindentation instruments used by the
participants were manufactured by Agilent, formerly MTS (USA),
Hysitron (USA), CSM (Switzerland), Micromaterials (UK) and
Fischer (Germany).
4.2. Materials and procedure
For the comparison, one set of specimens was used by all
participants. A tungsten specimen was provided for calibration of
the instrument frame compliance, and fused silica was provided
for determination of the area function of the indenter. The
comparison protocol called for the participants to use the methods
outlined in ISO 14577 to determine the instrument compliance and
indenter area function. Unlike in the rst comparison, (1 0 0)
aluminum was the single test piece chosen. Grids were engraved
on the specimens and each participant was assigned a location
within the grid to perform their indentations.
There were two possible ranges in which the participants could
perform measurements. The low force range was from 0.1 mN to
10 mN, and the high force range was from 10 mN to 100 mN. Based
on their instrument capabilities, some participants chose to
perform measurements over only one range, while others obtained
Table 9
Participants in CIRP comparison, 2009.
Physikalisch-Technische Bundesanstalt (PTB), Braunschweig (Germany)a
Oklahoma State University, Stillwater, OK (USA)a
CSM Instruments SA, Peseux (Switzerland)
ISTEC-CNR, Faenza (Italy)
Stiftung Institut fur Werkstofftechnik (IWT), Bremen (Germany)
Aristoteles University of Thessaloniki (LMTME), Thessaloniki (Greece)
Los Alamos National Laboratory, Los Alamos, NM (USA)
National Institute of Standards and Technology (NIST), Gaithersburg,
MD (USA)
National Physical Laboratory (NPL), Teddington (UK)
University of California, Berkeley, CA (USA)
Vlaamse Instelling vor Technologisch Onderzoek (VITO), Mol (Belgium)
Korea Research Institute of Standards and Science (KRISS), Daejeon (Korea)
a
Pilot participants.
813
Table 10
Maximum indentation forces for calibration and test piece.
Group
Maximum forces for

calibration (mN)
Maximum forces for

test piece (mN)
Low force
High force
0.1, 0.5, 1, 5, 10
10, 50, 100, 500, 1000
0.1, 1, 5
10, 50, 100
data for both ranges. Table 10 shows the maximum forces used for
the calibrations in tungsten and fused silica, and for the
measurements of hardness and elastic modulus of the (1 0 0)
aluminum test piece.
The loading function shown in Fig. 3 was prescribed in the
protocol and used by all participants. The loading function
consisted of: a 30 s loading, a 30 s hold at the maximum force,
unloading to 10% of the maximum force in 10 s, a 60 s hold at 10%
of the maximum force and a 2 s unloading to zero force. The drift
rate of the instrument was either determined from the last 50 s of
the hold period at 10% of the maximum force or prior to the start of
the indentation cycle. If the drift rate exceeded 0.1 nm/s the
indentation was excluded from the data set. A Berkovich diamond
indenter was used for all indentations. Ten indentations were
performed for each maximum load for both the calibrations and
the test piece measurement. The participants were asked to report
the plane strain indentation modulus, the indentation hardness
and the Martens hardness obtained for the (1 0 0) aluminum test
piece. The plane strain indentation modulus, is related to the
indentation modulus, given in Eq. (3), by the following:
EIT
EIT
1 ns 2
(16)
The indentation modulus of the (1 0 0) aluminum test piece was

calculated from the plane strain indentation modulus by assuming
a value for Poissons ratio of (1 0 0) aluminum, ns = 0.347 [79]. The
indentation hardness is given by Eq. (2), and the Martens hardness,
HM, is given by:
HM
F
AS hmax
(17)
where the surface area As(hmax) of the indenter is evaluated at the

maximum depth of indentation.
4.3. Results
The results obtained for the indentation modulus, indentation
hardness and Martens hardness for the (1 0 0) aluminum test piece
over the range of test forces are shown in Figs. 1719. The error
bars in the gures represent one standard deviation of the
measured data. Fig. 17 shows the results for indentation modulus
Fig. 17. Indentation modulus, EIT, obtained for the (1 0 0)Al test piece over the range
of forces investigated. The dotted line represents the value of elastic modulus
obtained by laser acoustic measurements on similarly prepared (1 0 0)Al.
Fig. 18. Indentation hardness, HIT, obtained for the (1 0 0)Al test piece over the
range of forces investigated.
obtained by the 12 participants, who are labeled anonymously. Also

shown as the dotted line, is the value of elastic modulus obtained by
laser acoustic measurements made at the PTB on similarly prepared
(1 0 0)Al which resulted in an elastic modulus of E = (70.6 1.4) GPa,
consistent with reported values for aluminum of 67 GPa to 71 GPa
[80]. At a test force of 0.1 mN, the indentation modulus appears to be
lower than the values obtained at the higher test forces. It is not clear
without further investigation as to whether this has a physical basis
or is a measurement artifact. Fig. 18 shows the results for indentation
hardness. The values for HIT are seen to increase at lower test forces
(i.e., lower depths of penetration). This observed indentation size
effect is consistent with other results obtained for aluminum [64] as
well as for a broad range of other materials. Only 9 participants
provided results for Martens hardness. These are shown in Fig. 19,
where the Martens hardness is also seen to exhibit the indentation
size effect.
The results for repeatability, the variation of the measurement
obtained by one participant, and the reproducibility, the variation
of the measurement between participants can be expressed by the
coefcient of variation, CV, as given by Eq. (11). The results
obtained for repeatability and reproducibility, in terms of the
coefcient of variation, for the indentation modulus and the
indentation hardness are shown in Figs. 20 and 21 respectively.
Also shown are the results obtained from the rst CIRP
intercomparison on steel. The repeatability CV shown in Fig. 20
is the average repeatability CV, as determined by the average of the
coefcients of variation, obtained for all contributing participants
at a given test force. The reproducibility CV shown in Fig. 21 is the
coefcient of variation obtained for the contributing participants at
a given test force. In the gures, test force is shown on a logarithmic
scale. At the high end of the test force range (100 mN) the
repeatability CV for indentation modulus of the (1 0 0) aluminum
Fig. 19. Martens hardness, HM, obtained for the (1 0 0)Al test piece over the range of
forces investigated.
814
Fig. 20. Repeatability CV of (a) indentation modulus and (b) indentation hardness
over the range of test forces investigated. Also shown are the results from the 1997
CIRP intercomparison on steel.
Fig. 21. Reproducibility CV of (a) indentation modulus and (b) indentation hardness
over the range of test forces investigated. Also shown are the results from the 1997
CIRP intercomparison on steel.
was found to be 0.05 compared to the low end of the range

(0.1 mN) where it was 0.14. The repeatability CV for indentation
hardness ranged from 0.03 up to 0.31. The reproducibility CV for
the indentation modulus at the high end range was 0.11 and
remained relatively constant for the complete force range. The
reproducibility CV for indentation hardness ranged from 0.11 to
0.22.
These results can be compared to those obtained on steel in the
rst CIRP comparison completed in 1997, also shown in Figs. 20
and 21. Although the test pieces in the comparisons were different,
the results show the tendency that the CVs for both repeatability
and reproducibility have improved in the last 1015 years. The CVs
for repeatability and reproducibility of both the indentation
modulus and indentation hardness are signicantly smaller in the
recently completed comparison when compared to the rst. The
improvement in repeatability CV is most likely due to improvements in the nanoindentation instruments including improved
design and measurement systems. The improvement in reproducibility CV is most likely due to the application of the standardized
test cycles and calibration procedures described in ISO 14577.
Based on the results of the recent comparison, the use of test forces
of F 1 mN for quality assurance applications appears to be now
possible. The results obtained from the recent comparison form a

solid basis for the introduction of procedures for the determination
of the uncertainty of nanoindentation measurements.
Table 11 shows the results for the repeatability CVs obtained
from the recent comparison on (1 0 0)Al, results from the rst
comparison obtained for steel and glass, and some recently
reported data for Ni and BK-7 which resulted from a study [38]
conducted to establish precision statements for ASTM E 2546-07.
The results for repeatability CV from the recent CIRP comparison
are greater than those obtained in the precision statement study,
however the CIRP comparison values represent averages of all
participating laboratories as compared to one laboratory which
conducted the precision statement study.
It should be emphasized that the repeatability or reproducibility as represented by the coefcient of variation does not equal
the measurement uncertainty, since it represents only the
stochastic part of the uncertainty. Although with the determination of the indenter area function with the reference material fused
silica and of the instrument compliance with the reference
material tungsten, essential systematic deviations of the instrument were characterized, not all important systematic inuence
quantities have been determined. Further, the development of a
Table 11
Repeatability CV obtained for indentation modulus and indentation hardness for a range of materials and test forces.
Test force (mN)
Indentation modulus
Indentation hardness
(1 0 0)Al [42]
Ni [38]
Steel [77,78]
Glass [77,78]
BK-7 [38]
(1 0 0)Al [42]
Ni [38]
Steel [77,78]
Glass [77,78]
BK-7 [38]
0.1
1
5
10
50
100
0.14
0.09
0.09
0.07
0.05
0.05
0.04
0.01
0.15
0.12
0.20
0.18
0.12
0.10
0.07
0.10
0.02
0.01
0.31
0.13
0.10
0.08
0.03
0.02
0.03
0.01
0.20
0.17
0.16
0.14
0.55
0.22
0.11
0.08
0.05
0.02
0.01
guideline for the estimation of the measurement uncertainty of the

instrumented indentation test is just being developed. Therefore in
these comparisons the common procedures used for the evaluation
of key comparisons were not yet applied.
Although the CVs for repeatability and reproducibility of the
recent comparison on nanoindentation were found to be better
than in the previous comparison, they are still much worse than
that in macro-hardness measurements where the CVs for
repeatability and reproducibility are typically a few percent. This
demonstrates the challenge for the further development of
nanoindentation.
5. Application areas
5.1. Derivation of tensile properties from IIT
s IT
1 F max
c Ac
eIT a tan g
material at the perimeter of the indentation. Other expressions for

the representative strain have been proposed; Ahn and Kwon [81]
found the above expression to best t tensile test results for a
variety of steels. In the third step of the iterative procedure, the
representative stress and strain are t to the equation sIT = KeITn
where K is the strength coefcient and n is the strain hardening
exponent. The value of n obtained from the curve t is compared to
the initial value of n and if they are different a new value of n is
assumed and the process repeated until convergence is achieved.
When convergence is achieved at a value of n = nIT, the plastic
region of the stressstrain diagram is determined. The elastic
behavior is characterized by the elastic modulus obtained from
Eq. (3). The strain at yielding, ey, can be determined by solving the
equation:
K ey nIT EIT ey 0:002
Accurate determination of tensile properties from IIT would

have signicant advantages over the traditional tensile test. In the
nano range, indentation testing measures a small volume of
material thus the tensile properties of small particles, coatings or
surfaces which have been treated (chemically, physically or
thermally) could be obtained. Indentation testing machines can
be made portable thus enabling in situ, on-site testing. Further
indentation testing is nearly non-destructive and there is relatively
little test sample preparation required. Monitoring of real
structures throughout their service life would be easier with IIT
and there would be no need for witness specimens as in the case of
traditional tensile testing.
The ISO Technical Report 29381 [39] summarizes the derivation
of tensile properties from IIT. Although in principal the methods
given in the report could be applied to all ranges of indentation
testing, it is recommended that maximum test forces in the range
of 2 N to 3 kN be used. The report describes three methods and the
main requirements, advantages and disadvantages of each are
presented. The three methods are: representative stress and strain,
Inverse FEA methods, and Neural networks. These methods
commonly use the instrumented indentation testing cycle, often
called the partial unloading method [13], which applies a
progressively increasing force but stops in a series of steps where
the force is partially removed to obtain the upper portion of the
force removal curve. This portion of the curve is used to obtain the
contact stiffness and contact depth at that force. The partial
unloading method allows a wide range of indentation sizes to be
performed at the same location. In all three methods, the complex
stress/strain eld beneath the indenter is simplied to a single pair
of stress and strain values, often called the representative stress
and strain. In the following each of the three methods is briey
presented.
In the representative stress and strain approach [8185] an
iterative procedure is used to determine the strain hardening
exponent, n, and the strength coefcient, K, of the test material. In
the rst step of the iteration procedure, a value of n is assumed and
using this value the pile-up or sink-in of material is calculated. By
using FEA to model the indentation process for a number of
materials both real and ctitious, the pile-up or sink-in was found
to be a function of n and the ratio hmax/R where R is the radius of the
indenter, i.e., hpile = f(n, hmax/R) [84]. The calculation of the pile-up
or sink-in enables the accurate determination of the contact depth
hc and contact radius a. In the second step of the iteration
procedure, the representative stress and strain are calculated, for
example, by the following equations [81]:
(18)
(19)
where c is a value which ranges from about 1.1 for elasticplastic

deformation up to about 3 for fully developed plastic ow. The
value a is a constant that was found to be 0.1 for a variety of steels
and g is half of the contact angle between the indenter and the test
815
(20)
where a 0.2% offset strain has been assumed. The yield strength can
then be calculated from this strain. The indentation tensile
strength, su,IT, can be calculated by setting eu = nIT in the equation:
s u;IT K eu nIT
(21)
The accuracy of the results obtained by the representative stress

and strain approach is greatly inuenced by the functional
relationship used in the determination of the pile-up or sink-in,
the value of c and the value of a in Eqs. (18) and (19). Although
good agreement between the properties derived by IIT and those
from the tensile test have been obtained for various materials or
groups of materials with similar stressstrain relationships, there
exists no universal values of the functions f, and c, and the value a
that will obtain suitable results for all materials. The representative
stress and strain approach is relatively easy to implement and
suitable for the tracking of material properties over time.
Inverse FEA methods [8690] attempt to solve the reverse
problem of obtaining tensile properties of the test material from
indentation test results. Although there has been some discussion
about the uniqueness of the solutions obtained for conical or
pyramidal indenters [91], under certain circumstances unique
solutions can be obtained [8689]. In the method developed by
Bouzakis et al. [86,87] the indentation test data of the loading
curve are processed in a stepwise fashion at a given spacing. For
each force-depth pair (Fi, hi) an FEA model is solved to obtain the
equivalent stress and strain that are consistent with this data point.
The series of equivalent stress and strain values are then used to
determine the tensile properties. Dao et al. [89] used dimensional
analysis and FEA to investigate a broad range of hypothetical
materials. They found that the yield strength was moderately to
signicantly sensitive to the input parameters. For example a 2%
change in the slope of the unloading curve at the maximum depth
produced a 22%/+16% change in the yield strength when the strain
hardening exponent n 0.1 and a 27%/+81% change in yield
strength for n > 0.1. Bucaille et al. [88] extended the model of Dao
et al. [89] to include indentations with indenters with different
included angles. The inverse FEA methods are typically computer
intensive and can obtain results for a broad range of materials.
The third method described in the technical report is a trained
neural network [9294]. The method presented in these papers
was used to study the behavior of viscoplastic materials however
the method could also be applied to other materials as well. The
method used solutions from FEA simulations of indentations to
train a set of neural networks. Each of the neural networks in the
set was used to solve for a particular variable or function. The set
includes neural networks to determine: the zero point correction,
the elastic modulus, the viscosity parameters, and the stressstrain
diagram. The method is capable of handling a wide range of
unknown materials however the results depend on the quantity of
the input data and the validity of the training process.
Table 12, reproduced from the ISO technical report [39],
compares the three methods and gives the relative advantages and
disadvantages of the methods.
816
Table 12
Comparison of methods for the derivation of tensile test properties from IIT [39].
Method 1: Representative stress and strain
Method 2: Inverse analysis by FEA
Method 3: Neural networks
Computational simulation
Possibility of using FEA to determine

pile-up, representative stress and strain
for development of the method
Inverse conical method

Dimensionless functions by forward
analysis using FEA
Inverse numerical method
Execution of FEA until simulation and
experiment results agree
Forward analyses using FEA for the

training of the neural networks
Experiments
Multiple loading and unloading with

a spherical indenter

Single indentations by sharp indenters
with various angles
Single indenting, proling residual
impression
Multiple creep loading and single

unloading with a spherical indenter
Analysis
Dening true stress and strain with

indentation parameters
Fitting to constitutive equation
Input of indentation curve to trained

neural networks given procedure
Equilibrium stressstrain curve
Tensile properties obtained:

sy,IT, su,IT, nIT
Input of indentation parameters to

dimensionless functions
Viscosity parameters obtained: overstress,

OS, viscosity exponent, m
Not needed (determination only from

FEA simulation)
Experimental evidence
6 metals in [81]
7 metals in [83]
2 metals in [82]
Round-robin test (RRT) completed
in Korea
2
5
4
6
Relative advantages
Deterministic algorithm
No need for computational simulations
Sufcient experimental verication
Application of any indenter

Flexible algorithm
Time dependency parameters

Flexible algorithm
Relative disadvantages
Rigid algorithm
Need for special software
Numerical estimation of parameters
Indispensable determination of
starting parameters
Need for special software (trained

neural networks)
Time-consuming test cycle
5.2. Indentation of biological materials

The indentation of biological materials presents unique
challenges as compared to the indentation of metals. In general
biological materials have a small elastic modulus, exhibit timedependent mechanical behavior and their behavior is often
dependent on their hydration state [95]. The small elastic modulus
of biological materials can lead to signicant difculties in
establishing the location of the test piece surface relative to the
indenter [96]. Kaufman and Klapperich [96] found in the
indentation of pHEMA hydrogels that errors in the determination
of the zero point could result in the indentation modulus being
underestimated by up to 30%. They suggest starting the indentation loading cycle from a location known to be above the surface
and then, after the indentation is complete, determining the
location of the surface from the force data.
Because of the viscoelasticplastic nature of many biological
materials, Menck et al. [97] have developed a method for the
indentation of these materials and the analysis of the resulting
data. A model of the test material can be constructed from springs,
dashpots and a plastic element as shown in Fig. 22. This model
consists of: the instantaneous elastic modulus, E0, instantaneous
hardness, H0, yield strength Y, compliance elements C0, C1, C2,
viscosity, hv, viscous compliance cv and retardation times t1, t2.
The model consists of two KelvinVoigt bodies which are modeled
as a spring and dashpot in parallel. These two are in series with the
Fig. 22. Viscoelasticplastic model with spring, plastic element, dashpot, and two
KelvinVoigt bodies. C0, C1, C2 are compliances, E0 and H0 are instantaneous elastic
modulus and hardness, Y is yield strength, hv is viscosity, cv is viscous compliance
and t1, t2 are retardation times [97].
metals in [89]
metals in [88]
metals in [90]
ceramic and coating [86]
3 metals in [92]
4 metals in [93]
other elements. This model can be modied for a particular

application by adding or removing elements as needed.
To determine the constants in the viscoelasticplastic model
shown in Fig. 22 a special test force vs. time cycle is recommended.
The cycle is shown in Fig. 23 and is composed of a rapid loading to
the maximum test force, a long hold at this force, rapid unloading
to a very low force, a long hold at this force, and an unloading to
zero force. The rst hold period is used to determine the constants
in the model and the second hold period is used to conrm these
results and rene the model if necessary. The times of the
individual parts of the cycle will depend on the material being
tested. In the indentation of dental enamel with a maximum load
of 250 mN, the loading and unloading occurred in 20 s and the hold
periods were about 1000 s [97]. The results of the indentation test
are evaluated as follows. For the rst hold period the indentation
depth and force data are t to the following equation for the model
shown in Fig. 22:

t
t
2
h t FK C B cv t D1 exp
D2
(22)
t1
t2
where h: indentation depth; t: time; F: indentation force; KC:

geometric constant from indenter shape; cv: viscous compliance;
Fig. 23. Test force vs. time cycle for the indentation of viscoelasticplastic materials
such as biological materials.
t1, t2: retardation times; and

B C0
cv tR
C1 C2
2
D1;2 C 1;2 r1;2
(23)
(24)
with C0: instantaneous compliance; tR: time of loading; C1, C2:

compliance; r1, r2: ramp correction function.
In Eq. (22), the rst term in the square brackets corresponds to
the spring, the second term to the dashpot, and the third and fourth
terms to the KelvinVoigt elements. From the tting of Eq. (19) the
constants B, cv, D1, D2, t1 and t2 are determined. The ramp
correction factors can then be computed from [98]: r1,2 = (t1,2/
tR)(exp(tR/t1,2) 1). The constants C1, C2 can be computed from
Eq. (24). Lastly Eq. (23) is used to compute C0. This procedure can
be used for models with a different number of elements and/or
different elements and the results then compared to the measured
data to obtain the model that best ts the data. Further it is
suggested [97] that curve tting of the results of the second hold
period can be used to help decide the most appropriate model.
In addition to the above described quasi-static indentation
method, dynamic indentation methods can also be used to
evaluate viscoelastic materials. In dynamic indentation a small
oscillating force is superimposed with the quasi-static force
applied to the test piece. Typically the force oscillation produces
a depth oscillation which is less than 5 nm peak to peak. In
viscoelastic materials there is a phase difference between the
oscillating force and the oscillating depth. This phase difference is
used in the calculation of the loss modulus and storage modulus,
which are related to the energy that is dissipated or stored by the
test piece. Fig. 24 shows a model of the indentation test machine
and test piece used in the analysis of dynamic indentation. The test
piece is represented by the spring, ST and the dashpot, CT. The test
machine is represented by the spring, Km, dashpot, Cm and
oscillating mass, m. Analysis of this model leads to the following
equations for the storage modulus (E0 ) and loss modulus (E00 ) [99]:
p

p F0
cos f
(25)
E0 p
2 A h0
p

p F0
E00 p
sin f
2 A h0
817
their mechanical properties. For example, teeth in the wet

condition were found to have a hardness value approximately
1/3 and an indentation modulus approximately 1/2 of the values
obtained for dry teeth. This group further explored the use of
different indenter geometries on the indentation modulus of
dental enamel [103]. They found that for dry enamel indentation
modulus values between 55 and 60 GPa were measured for all
indenters. However for wet enamel they found that the cube
corner indenter produced lower values of indentation modulus.
They suggest that a different deformation mechanism results with
the sharp cube corner indenter. Akhtar et al. [104] combined
nanoindentation with uorescence microscopy to study the aorta
and vena cava of ferrets. Fluorescence microscopy was used to
identify the ber distribution in the blood vessels, and nanoindentation was used to measure the indentation modulus. The
modulus of the aorta in cross section was found to range from
about 7 GPa at the innermost wall to about 35 GPa at the
outermost wall. The modulus of the vena cava was found to range
from about 20 GPa to 35 GPa with the higher values occurring at
the innermost and outermost surfaces and the lower values in the
middle. Bouzakis et al. [106] combined indentation with an FEM
based model to obtain the stressstrain curve for lumbar spine
vertebrae. They found an elastic modulus of approximately 13 GPa,
a yield strength of 60 MPa and a maximum strength of 94 MPa.
Tong et al. [107] studied the elastic modulus and hardness of the
stigma of dragonies using nanoindentation. The stigma of a
dragony is located near the end of the wing and is important to
balance the center of mass of the dragony and to stabilize high
speed ight. Fig. 25 shows a photograph of a dragony Anax
parthenope julius Brauer with a wingspan of approximately 97 mm
and a close-up of a stigma which has been removed from the wing.
The indentation modulus was found to range from about 1 GPa to
3 GPa and the hardness varied from 350 MPa to 50 MPa. The
highest values of modulus and hardness were obtained from
location 1 in Fig. 25.
The indentation testing of biological materials has been, and
continues to be, of signicant interest. Standards in the testing of
viscoelastic materials which includes many biological materials
are currently lacking. Recently however there has been some work
in this area [40] to address this deciency.
(26)
where F0 is the amplitude of the oscillating force, h0 is the

amplitude of the oscillating depth, A is the contact area and f is the
phase angle between the force and the depth. In Eqs. (25) and (26)
the dynamic response of the test machine has already been taken
into consideration. In a comparison with traditional rheological
techniques it was found that dynamic indentation produced
similar results for materials with high energy storage but
signicantly different results for materials with high energy
dissipation [101].
Instrumented indentation has been used to quantify the
behavior of a variety of biological materials including dental
enamel [97,102,103], blood vessels [104], bone [105,106] and the
wings of dragonies [107,108]. Guidoni et al. [102] found that the
storage and hydration of teeth can have a signicant inuence on
Fig. 24. Model of indentation test machine and test piece used in the analysis of
dynamic indentation. After [100].
Fig. 25. Photograph of dragony Anax parthenope julius Brauer (a) and detailed view
of the stigma (b). The location of the stigma on the wing of the dragony in (a) is
denoted by a rectangle. Location of indentations given by numbers. After [107].
818
6. Conclusions
We have presented a review of the measurement methods used
in nanoindentation, the instruments currently in use, and the
procedures for the analysis of the resulting data. The methods
developed for verication and calibration, including a discussion
on uncertainty of parameters were presented. The results of the
most recent CIRP sponsored comparison on nanoindentation were
presented and compared to the results obtained in the rst such
comparison. Two examples of some emerging uses of the
technique, namely determination of materials tensile properties,
and investigations of biological materials were discussed.
Although the ISO standards for the instrumented indentation
testing of bulk materials were published in 2002, it is still not
uncommon to nd published papers that do not follow the
standards. The use of the standards in the 2009 CIRP sponsored
comparison on nanoindentation contributed to the improvement
of reproducibility in the measurement of the indentation modulus
and indentation hardness when compared to the results of the
1997 CIRP sponsored comparison. In the emerging areas of
instrumented indentation for the derivation of material tensile
properties and the testing of biomaterials, currently no standards
exist, however work on developing standards in these areas is ongoing. With the adoption of standards in these emerging areas
improvements in the reproducibility of results are expected.
Acknowledgements
The authors would like to thank Drs. R. Hocken, G. Goch, W.T
Estler, K.-D. Bouzakis, Yu. Golovin, T. Chudoba and all those who
have provided materials for and thoughtful review of this
contribution. We would also like to thank the participants in
the recent CIRP sponsored comparison for their signicant efforts
to make it a fruitful exercise. We thank the University of North
Carolina at Charlotte and the PTB in Braunschweig for assistance
with the comparison. Additional thanks are extended to the
ofcers of the CIRP Scientic Technical Committee STC S, Drs. A.
Balsamo, H. Hansen and H. Haitjema for their help and support of
this work.
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Measuring Methods and Applications of Nanoindentation

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CIRP Annals - Manufacturing Technology 59 (2010) 803819

Contents lists available at ScienceDirect

CIRP Annals - Manufacturing Technology

Nanoindentation: Measuring methods and applications

century, instruments which measured indentation depth under

Instrumented indentation testing (IIT) has emerged as an

D.A. Lucca et al. / CIRP Annals - Manufacturing Technology 59 (2010) 803819

1.2. Standards and international comparisons

improvements in the indentation instruments a second CIRP

Fig. 1. Geometry of Vickers indenter, left, and Berkovich indenter, right.

D.A. Lucca et al. / CIRP Annals - Manufacturing Technology 59 (2010) 803819

Fig. 2. Berkovich indenter measured by a metrological atomic force microscope.

Berkovich indenter however the angle between the axis of the

D.A. Lucca et al. / CIRP Annals - Manufacturing Technology 59 (2010) 803819

Picodentor HM500 (Fischer)

measurement systems used include electromagnetic, capacitive

With optional head.

D.A. Lucca et al. / CIRP Annals - Manufacturing Technology 59 (2010) 803819

where e is 0.75 for a Berkovich or Vickers indenter. With knowledge

where ns is Poissons ratio of the test piece; ni is Poissons ratio of

another axis of motion and thus enable the instrument to perform

where G is the gamma function. For many materials m is in the

2.3. Analysis of data

The basic analysis of instrumented indentation data has its

where f is the half-included angle of the indenter. For a Berkovich

Chudoba and Jennett arrived at a similar result by considering a

D.A. Lucca et al. / CIRP Annals - Manufacturing Technology 59 (2010) 803819

Indentation modulus, EIT

Indentation Hardness, HIT

indentation depth is used, Martens hardness includes the elastic

orientations of ZnO, (0 0 0 1) and 1 0 1 0. In both cases the

D.A. Lucca et al. / CIRP Annals - Manufacturing Technology 59 (2010) 803819

are performed at a minimum of three different, and preferably ve

indentation depths should be selected such that the indentation

Optical microscopy, AFM

D.A. Lucca et al. / CIRP Annals - Manufacturing Technology 59 (2010) 803819

provided. The geometry of the indenter should be veried so that it

sensor is most commonly used. The measuring system must be

D.A. Lucca et al. / CIRP Annals - Manufacturing Technology 59 (2010) 803819

E  70 GPa. To begin the procedure a series of indentations in the

using the value of Cf estimated from Eq. (8). An area function,

More recently however, truncated forms of this equation have

where s(q) is the experimental standard deviation and q is

Hardness, HM or HIT (MPa)

Indentation modulus, EIT (GPa)

Micro range h > 1 mm

tory if it meets the requirements given in Table 7. It should be

where k: coverage factor of expanded uncertainty (k = 2); uRMx:

D.A. Lucca et al. / CIRP Annals - Manufacturing Technology 59 (2010) 803819

where s(xk) is the experimental standard deviation of n repeated

where the measured value y is a function of input variables xi such

Relative combined uncertainty (%)

was available having been developed at three or four research

D.A. Lucca et al. / CIRP Annals - Manufacturing Technology 59 (2010) 803819

Maximum forces for

Maximum forces for

The indentation modulus of the (1 0 0) aluminum test piece was

where the surface area As(hmax) of the indenter is evaluated at the

obtained by the 12 participants, who are labeled anonymously. Also

D.A. Lucca et al. / CIRP Annals - Manufacturing Technology 59 (2010) 803819

was found to be 0.05 compared to the low end of the range

possible. The results obtained from the recent comparison form a

E 70 GPa. To begin the procedure a series of indentations in the