Nanomechanical Characterization of Materials by

FEATURE Nanoindentation Series

CONTINUOUS STIFFNESS MEASUREMENT DURING

INSTRUMENTED INDENTATION TESTING
by J. Hay, P. Agee, and E. Herbert

nstrumented indentation testing (IIT) is a technique Table 1—Summary of common terms

I for measuring the mechanical properties of materials.

This is the second article in this ET feature series on
the topic. The first article was a review of common
terminology as well as basic procedures and analyses.1 This
article introduces an advanced form of IIT that was developed
SYMBOL DIMENSIONS

P F
TERM RELEVANCE

Semistatic force Semistatic force exerted by

the indenter on the
sample and vice versa
by Dr. John Pethica and Dr. Warren Oliver about 20 years
ago.2,3 h L Semistatic Semistatic penetration of
displacement the indenter into the test
During basic IIT, contact force and penetration are measured material, relative to the
position at which the
continuously as a hard indenter is pressed into contact
indenter first contacted
with, and then withdrawn from, a test material. Continuous
the surface
stiffness measurement (CSM) also involves pressing an
indenter into contact with a test material while continuously F(t) F Force function Oscillating force,
superimposed upon
measuring contact force and penetration. But in addition,
semistatic force
a small oscillation is superimposed on the semistatic force,
and a frequency-specific amplifier is used to measure the z(t) L Response Oscillation of the indenter
function as a consequence of F(t)
response of the indenter. Typically, the amplitude of the force
oscillation is controlled (increased) such that the amplitude Fo F Force amplitude Amplitude of F(t)
of the displacement oscillation remains constant. The ability zo L Displacement Amplitude of indenter
to superimpose an oscillation and measure the response buys amplitude oscillation, z(t)
a number of benefits over basic IIT. These benefits include: ω T−1 Angular Oscillation frequency
frequency
t T Time Abscissa for force and
• The ability to measure mechanical properties as a
response functions
continuous function of distance into the surface (depth
(semistatic and oscillating)
profiles of properties), as in Ref. [4],
φ – Phase angle Angle by which the
• The ability to measure storage and loss modulus of
response function z(t) lags
polymers as a function of frequency,5 – 7
the force function F(t)
• Improved in situ surface detection, and
• Alternate imaging modes when the indentation system m FT2 L−1 Mass
is used as a profilometer D FTL−1 Damping
K FL−1 Stiffness
i Subscript: of the indenter
In this article, we first explain the technique in detail. Then,
we explain how CSM is used to measure properties as a c Subscript: of the contact
continuous function of penetration depth. Other applications e Subscript: effective
of CSM will be reserved for future articles of this series. f Subscript: of the frame
Terminology is often a significant barrier to understanding act Subscript: actual
a new technique. Therefore, a summary of CSM terms are init Subscript: initial
provided in Table 1. Variables that are common to basic IIT
(such as force and displacement) are represented with the
same symbols that were used in the first article.
THE SIMPLE-HARMONIC OSCILLATOR
Editor’s Note: This article is part of the ET Feature Series on Nanomechanical A simple-harmonic oscillator comprises three basic compo-
Characterization of Materials by Nanoindentation (instrumented indentation nents: a spring of stiffness K, a mass m, and a dashpot
testing) which lends itself to testing small volumes of material. This series features
articles describing the main experimental technique(s), background theory and with damping coefficient D. It is beneficial to review the
data reduction, testing of polymers, and low-k thin films. Additionally, most recent analysis of this system, illustrated in Fig. 1, before applying
developments in these techniques will be addressed throughout the series. Series it to an indenter. If this system is excited by an oscillating
editor: Ibrahim Miskioglu, Michigan Technological University.
force, F (t) = F0 eiωt , then we expect a response of the form
J. Hay (jenny.hay@agilent.com) and P. Agee are application engineers with z(t) = z0 ei(ωt−φ) ; that is, we expect the oscillation of the mass
Agilent Technologies, Nanotechnology Measurements Operation. E. Herbert (SEM
member) is a postdoctoral researcher with the Department of Material Science and to be at the same frequency, ω, but lag by a phase angle, φ.
Engineering, University of Tennessee, Knoxville. The second-order differential equation which describes the
doi: 10.1111/j.1747-1567.2010.00618.x
May/June 2010 EXPERIMENTAL TECHNIQUES 86 © 2010, Society for Experimental Mechanics
CSM DURING INSTRUMENTED INDENTATION TESTING

K D Fo /zo
Dw

f
x
K-m w2

m
Fig. 2: Illustration of solution for system of Fig. 1
z(t) = z0ei(wt-f)
F(t) = F0eiwt This solution is illustrated in Fig. 2; by Pythagorean’s
theorem, we can also express the solution as
 2
2 2 Fo
(K − mω ) + (Dω) = 2
. (10)
Fig. 1: Simple-harmonic oscillator model zo

relationship between force and response is: The dynamic compliance, zo /Fo , is the ratio of the amplitude
mz̈(t) + D ż(t) + Kz(t) = F (t). (1) of the displacement oscillation to the amplitude of the
excitation; it has the dimensions of length per unit force.
Taking the first and second derivatives of z(t) yields If the system is underdamped, this ratio peaks at resonance;
for frequencies greater than the resonant frequency, the
ż(t) = z0 iωei(ωt−φ) , (2) value of this ratio decreases monotonically with frequency.
z̈(t) = −z0 ω2 ei(ωt−φ) . (3) Solving Eq. 10 for dynamic compliance yields
Substituting the expressions for z, z’, z’’, and F into Eq. 1 zo 1
yields =  (11)
Fo 2 2
(K − mω ) + (Dω) 2
−mz0 ω2 ei(ωt−φ) + Dz0 iωei(ωt−φ) + Kz0 ei(ωt−φ) = F0 eiωt .
(4)
Multiplying every term in Eq. 4 by eiφ /(z0 eiωt ) yields MODELING THE INDENTER ALONE
F0 iφ Let us first apply this model to an indenter that is hanging
−mω2 + iDω + K = e , (5)
z0 free. When the indenter is not in contact, the model
components are those of the indenter alone: K = Ki , m = mi ,
and invoking Euler’s rule to substitute for eiφ yields
and D = Di . The springs supporting the indenter shaft are
F0 the primary contributors to Ki . If capacitive plates are used
−mω2 + iDω + K = (cos φ + i sin φ). (6) for sensing or actuation, they are the primary contributors
z0
to Di . Finally, the mass of indenter shaft is the primary
Equating the real parts of Eq. 6 yields contributor to mi . Applying Eqs. 7, 8, and 11 to the case of a
F0 free-hanging indenter yields
K − mω2 = cos φ, (7) 
z0 F0 
Ki − mi ω2 = cos φ  , and (12)
and equating the imaginary parts yields z0 f ree−hanging

F0
Dω = sin φ. (8) 
z0 F0 
Di ω = sin φ  . (13)
So the phase angle, φ, by which the response lags z0 f ree−hanging
the excitation depends on the components through the
relationship
zo 1
Dω =  (14)
tan φ = . (9) Fo 2 2
K − mω 2 (Ki − mi ω ) + (Di ω) 2

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CSM DURING INSTRUMENTED INDENTATION TESTING
Logistically, a frequency-specific amplifier (i.e., a ‘‘lock-in
amplifier’’) is used to set the amplitude (Fo ) and frequency
(ω) of the excitation, and also to measure the amplitude
of the displacement response (zo ) at the same frequency as
well as the phase shift (φ ) between the two signals. Thus,
one way to determine values for the dynamic components
of the indenter is to oscillate it over a range of frequencies,
plot compliance versus frequency, and curve fit the data
using the form of Eq. 14, with Ki , mi , and Di as best-fit
constants. Such a plot is shown in Fig. 3. That the functional
form of Eq. 14 fits the data so well is evidence that the
simple-harmonic oscillator is a good model for the indenter.
The value for mi determined in this way is a sufficient
determination of the effective mass of the indenter. But Ki
may be a weak function of indenter position (if springs are
not perfectly linear), and for indenters that use a three-
plate capacitive gage, Di is a strong function of indenter
position. So historically, Ki and Di have been determined
a priori as a function of indenter position using secondary
calibrations. However, we shall see shortly that this is not
necessary.
The fact that the indenter behaves as a simple-harmonic
is not an accident, but a design criteria for indenters that
use this technology. Simple-harmonic behavior requires
that the motion occur in only one dimension, with only one
mode of oscillation. Atomic-force microscopes (AFMs) that
use cantilevered probes for scanning and indentation do
not meet these requirements. Thus for an AFM, modeling
the dynamic behavior of the indenter—an essential aspect
of obtaining quantitative dynamic results—is a much more
complicated prospect.
0.1
0.01
Compliance, m/N
0.001
0.0001
0.00001
1 10
Frequency, Hz
Fig. 3: Measured compliance and best fit to Eq. 14 for the Agilent G200 Nanoindenter (XP head). Compliance
was measured with the indenter hanging free in the center of its range of travel. Best fit values are
Ki = 92.02 N/m, mi = 11.6 g, Di = 2.66 N-s/m
88 EXPERIMENTAL TECHNIQUES May/June 2010
The resonant (or natural) frequency of the indenter in its
free-hanging state is (Ki /mi )1/2 . In dynamic indentation, a
higher natural frequency is advantageous for at least two
reasons:
• Building noise due to foot traffic, ground motion,
ventilation, and so on tends to be at frequencies less
than 10 Hz, so operating at frequencies above this range
decreases sensitivity to these noise sources.
• A larger frequency range is available for testing
samples for which behavior is expected to depend on
frequency.
Increasing the natural frequency can be achieved either
by increasing the stiffness of the supporting springs, or by
decreasing the mass of the indenter. However, increasing
the stiffness of the supporting springs is experimentally
disadvantageous, as it makes the indenter less sensitive.
So the best way to increase the natural frequency of the
machine is to decrease the mass. Therefore, users should
expect trends in hardware miniaturization to continue for
the dynamic advantages of a smaller moving mass.
MODELING THE INDENTER IN CONTACT
WITH A SAMPLE
Now, let us consider the situation when the indenter is in
contact with the test material. Components representing
the sample have been included in the model shown in
Fig. 4: Kc and Dc represent the stiffness and damping
of the contact, respectively. More complex models for the
contact have been proposed in an attempt to better model
real materials, but the practical benefit of the added
measured
best fit
100 1000
CSM DURING INSTRUMENTED INDENTATION TESTING

F0
De ω = sin φ. (20)
z0
Substituting expressions for Ke (Eq. 19) and Ki (Eq. 12) into
Eq. 17 yields the following expression for Kc :
  

Kf Fz 0 cos φ − Fz 0 cos φ 
Kf 0 0 f ree−hanging
Kc =   . (21)
F0 F0 
Kf − z cos φ − z cos φ 
Kc Dc Ki Di 0 0 f ree−hanging

In other words, the contact stiffness depends only on the

contact

frame stiffness and the real part of the amplitude ratio,

less the value of that same parameter just before contact.
One does not even need to know the mass of the indenter!
(Procedures for obtaining Kf should be provided by the
equipment manufacturer.) If the frame is infinitely stiff
mi relative to the stiffness of the contact (which may be an
appropriate assumption for small contacts or very compliant
z(t) = z0ei(wt-f) materials) then Eq. 21 simplifies further to

F(t) = F0eiwt F0 F0 
Kc = cos φ − cos φ  . (22)
z0 z0 f ree−hanging

Analogously, we calculate the damping of the contact as

Fig. 4: Model accommodating both instrument
and contact
complexity has yet to be demonstrated.8 When the indenter
is in contact, we must account for the elastic stiffness of
the frame with the component, Kf . Components of the
equipment and the contact may be combined and represented
by effective components such that we can continue to
use the simple-harmonic oscillator of Fig. 1, with K = Ke
and D = De ; we continue to represent the mass as mi ,
because the effective mass is not significantly affected by
contact. (For AFMs, the assumption that the effective mass
is not significantly affected by contact is probably not a
good one. Because the indenter mass is so small, the
mass of the deformed material may make a significant
contribution.) So the effective components are related to
the components representing indenter, frame, and contact
by
Ke = [1/Kf + 1/Kc ]−1 + Ki , and
De = Di + Dc .
Rearranging these equations to solve for the desired
components (the stiffness and damping of the contact) yields
Kf (K e − Ki )
Kc =
Kf − (K e − Ki )
(or Kc = Ke − Ki when Kf  Ke ) and
Dc = De − Di .
Invoking Eqs. 7 and 8 yields
F0
Ke − mi ω2 = cos φ, and
z0

F0 F0 
sin φ 
Dc = sin φ − . (23)
z0 z0 f ree−hanging
The contact damping is determined dynamically from the
imaginary part of the amplitude ratio, less the value of that
same parameter just before contact.
In school, one practices the analysis of oscillating systems
as a function of frequency; the resonant frequency for the
system is a fixed value, and one examines the response of
the system over a range of interesting frequencies relative
to the natural frequency. However, with a CSM test, it is
often the case that the excitation frequency is fixed and
the components (of the oscillator) change over the course
of a test, because of the contact changes. Let us say
that we excite the system at a frequency that is greater
than the natural frequency for the indenter in its free-
hanging state. As the indenter contacts the sample and
(15) is pushed into it, the effective stiffness of the oscillator
increases, and so the natural frequency of the system (the
indenter together with the contact) increases. The system
(16) goes through resonance when the natural frequency passes
through the excitation frequency. (Thus, the indenter ought
to be critically or overcritically damped, so as to avoid a
sharp increase in oscillation amplitude at resonance.) If the
excitation frequency is lower than the natural frequency of
the indenter in its free-hanging state, then the system will
not go through resonance as a result of contact.
(17) The user should keep this dynamic behavior in mind when
setting parameters for an experiment. When using CSM
(18) to measure the properties of elastic-plastic materials as
a function of penetration depth (as we have done in this
work), the results should be independent of frequency, so
any convenient excitation frequency may be used within
the range of 0.5 ωn –5 ωn , where ωn is the resonant (or
(19)
natural) frequency of the free-hanging indenter. However,

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CSM DURING INSTRUMENTED INDENTATION TESTING
there are some applications of CSM for which it is
particularly advantageous to operate around resonance,
primarily because the phase angle, φ, changes dramatically
in this regime, and so it can be used as an ultrasensitive
measurement. If operating around resonance is desirable,
then one should control the excitation frequency and/or
contact force so that resonance is achieved. One use of
this strategy is sensitive contact detection. If the excitation
frequency is set just above the natural frequency of the free-
hanging indenter, then contact can be sensitively detected
based on change in phase angle. A similar strategy may be
used when the indenter is used as a profilometer for surface
imaging. Strong contrast in phase is obtained by setting the
excitation frequency just above the natural frequency, and
then selecting the scanning force so that the phase angle is
in the middle of its range.
GENERAL USE OF KC AND DC
Once Kc has been determined, either by Eq. 21 or Eq. 22,
it is used in place of the semistatic contact stiffness, S, in
all IIT calculations. (For a review of these calculations, the
reader should consult the first article in this feature series.)
So, the contact depth is calculated as
hc = h − εP /Kc , (24)
where h is the total penetration depth, ε is a geometric
constant, and P is the applied load. The contact area, A, is
calculated as a known function of the contact depth, hc . For
a Berkovich indenter, this calculation is
A = 24.56h2c + Chc , (25)
where C is a constant that is determined empirically by
indenting a known material, usually fused silica. For most
Berkovich indenters manufactured today, C has a value of
about 150 nm. Hardness is calculated as
H = P /A, (26)
so hardness depends on contact stiffness through the
calculation of contact area by Eqs. 24 and 25. (We note this,
because it is not necessarily obvious that the contact stiffness
must be known to determine hardness by an IIT test.) The
reduced modulus, Er , is calculated as
√ h / h—the displacement rate divided by the displacement.
π Kc
Er = √ (27)
2 A
If the response of the material is instantaneous (or
approximately so), then one should expect the results
obtained by CSM and semistatic testing to agree well. This
is the case for most metals, glasses, and ceramics. However,
if the response of the material occurs over time, then the
slope of the force-removal curve cannot be used to determine
contact stiffness, because the slope does not represent linear-
elastic recovery. This is the case for most polymers. For
such materials, CSM must be used to accurately measure
stiffness.
90 EXPERIMENTAL TECHNIQUES May/June 2010
APPLICATION: THIN COATINGS ON
SUBSTRATES
By far the most common application of CSM is in the
evaluation of thin coatings on substrates. Eqs. 26 and 27
are used to calculate hardness and Young’s modulus, so
that every test yields properties as a continuous function
of penetration depth. Without CSM, hardness and Young’s
modulus can only be realized at the maximum penetration
depth.
Experimental Method
To illustrate the utility of CSM, we tested a 200-nm gold
coating deposited on mica (layered silicate). We used an
Agilent G200 Nanoindenter fitted with a diamond Berkovich
indenter. We performed 10 semistatic tests according to
the method prescribed by ISO 14577.9 Each semistatic
test was performed to a different peak force to reveal
functionality with depth. Also, we performed eight CSM
tests, each to a peak depth of 1600 nm. For the CSM tests,
the excitation frequency was 45 Hz. (The values of mass and
stiffness obtained by fitting the data of Fig. 3 give a natural
frequency of about 14 Hz.) The excitation amplitude was
controlled such that the displacement amplitude remained
constant at 2 nm. For all tests, a Poisson’s ratio of 0.35
was used to calculate Young’s modulus from reduced
modulus.
The two types of tests (ISO 14577 vs. CSM) used substan-
tially different loading algorithms. Figure 5 compares the
force-time histories for two tests on the gold film—one ISO
14577 test and one CSM test. For all ISO 14577 tests, the
loading time was 30 s, the dwell was 15 s, and the unloading
time was 30 s. But for the CSM tests, force was applied such
that
1 dP
P  /P ≡ = constant (28)
P dt
until the peak displacement was achieved. In other words,
when the applied force was small, the force application rate
was also small; as the applied force increased, so did the
force application rate. We call the term on the left-hand side
of Eq. 28 the ‘‘indentation strain rate’’ or just ‘‘strain rate.’’
Strain rates of 0.05/s to 0.2/s are typically used. Because
the CSM method does not make use of data acquired during
unloading, any convenient algorithm may be used to remove
force. (To be consistent with other types of mechanical
testing, the indentation strain rate would be defined as
And in fact, such a definition would be advantageous for
displacement-controlled instruments. However, for materials
with a uniform hardness, P  /P is directly proportional
to h / h. This is proven by starting with the definition of
hardness, then differentiating both sides of the definition
with respect to time, and finally dividing by the original
definition. Therefore, from an analytic standpoint, it does
not matter whether one defines strain rate as P  /P or h / h.
But from a practical standpoint, if the instrument is force
controlled, it is much simpler to control P  /P .)
When performing a CSM test with a Berkovich indenter,
there are two advantages to holding the strain rate constant
CSM DURING INSTRUMENTED INDENTATION TESTING

200
180
160 CSM test
Load on surface (mN)
ISO 14577 test
140
120
100
80
60
40
20
0
0 50 100 150 200 250
Time (sec)

Fig. 5: Comparison of force-time algorithms used for CSM and ISO 14577 tests

during loading. The first reason is for good control of the CSM
amplitudes. The amplitude of the CSM force oscillation is
continuously adjusted so that the amplitude of the resulting
displacement oscillation remains constant at a small value
(≤2 nm). This control is more challenging when the rate
of change of stiffness is high. Figure 6 shows stiffness as
a function of applied force for one test on the gold film.
Because the rate of change of stiffness is very high when
the applied force is small, better CSM control is achieved
by loading slowly at the start of the test and faster as the
test proceeds. (One might wonder what loading rate is used
when the indenter first touches the surface, when P is zero
and P  /P is undefined. Actually, the loading rate required
to move against the support springs during the approach is
used until P  /P is well defined.)
The second reason for holding the strain rate constant is
to achieve a meaningful measure of hardness when testing
materials for which the response to an applied stress occurs
over time. For materials that manifest viscoplasticity (i.e.,
creep), Lucas and Oliver demonstrated hardness to be
a function of indentation strain rate.10 Specifically, they
measured the hardness of indium at five different strain
rates (P  /P ). The lowest strain rate yielded the lowest value
of hardness and the highest strain rate yielded the highest
value of hardness. Lucas and Oliver used this functionality
to determine the stress-exponent for creep of indium by
indentation to be 7.3. This is in good agreement with the
value as measured uniaxially by others.11 As previously
mentioned, CSM is often employed because the material is
strain-rate sensitive. Therefore, it is good practice to use
constant-strain-rate loading in combination with CSM.
Constant-strain-rate loading is a slower test. Therefore,
data are more likely to be affected by thermal drift, and
if the material exhibits viscoelasticity or viscoplasticity

600000
CSM contact stiffness (N/m)

500000 Test 3

400000

300000

200000

100000

0
0 20 40 60 80 100 120 140 160 180 200
Load on sample (mN)

Fig. 6: Stiffness versus load for a single test on a 200-nm gold coating. Rapid increase in stiffness at small forces
necessitates a constant-strain-rate loading algorithm to maintain the response oscillation at a constant value

May/June 2010 EXPERIMENTAL TECHNIQUES 91

CSM DURING INSTRUMENTED INDENTATION TESTING

(creep), then displacements cannot be corrected by observing
the displacement rate during a hold segment. That is, the
standard thermal-drift correction cannot be used. Therefore,
when using constant-strain-rate loading, it is important to
make sure that the thermal drift rate is low before initiating
testing. A rate of 0.05 nm/s or lower is recommended. The
drift criteria for constant-loading-rate tests can be more
lax—0.2 nm/sec is acceptable.
The oscillation amplitudes of the CSM option have non-
negligible effects on the semistatic measurements of force and
displacement.12 Thus, the initial measurements of semistatic
force and displacement (Pinit and hinit , respectively) were
corrected as follows:
Pact = Pinit + Fo , (29)
and
hact = hinit + Zo
where Pact and hact are the corrected values of semistatic
force and displacement, respectively.
RESULTS
Figure 7 shows the properties as measured by eight different
CSM tests; one CSM test is shown in black to make
it more visible. For comparison, properties as measured
semistatically according to ISO 14577 are shown as red
circles; each red circle is the outcome of one complete
semistatic indentation test. The semistatic results are in
good agreement with the CSM results, but CSM offers a
more complete picture of what is happening. The expected
modulus of gold is between 71 and 79 GPa, and the
expected modulus for mica (normal to the layers) is 60 GPa.13
Thus, the modulus gradually decreases from that of the gold
to that of the mica. With respect to hardness, we see it
increasing with depth from that of the gold to that of the
(30) mica. The results for displacements of less than 60 nm are

(a)
100
90
80
Test 001
70 Test 002
Modulus (GPa)

Test 003
60 Test 004
50 Test 005
Test 006
40 Test 007
30 Test 008
ISO Results
20
10
0
0 200 400 600 800 1000 1200 1400 1600
Displacement Into Surface (nm)

(b)
10
9
8
Test 001
7 Test 002
Hardness (GPa)

Test 003
6
Test 004
5 Test 005
Test 006
4 Test 007
3 Test 008
ISO Results
2
1
0
0 200 400 600 800 1000 1200 1400 1600
Displacement Into Surface (nm)

Fig. 7: For a 200-nm gold coating on mica, (a) modulus and (b) hardness versus indenter penetration depth by
means of CSM and semistatic testing according to ISO 14577. One CSM test yields a single gray (or black) trace.
One ISO 14577 test yields a single red point

92 EXPERIMENTAL TECHNIQUES May/June 2010

CSM DURING INSTRUMENTED INDENTATION TESTING

200
180
Load on sample, mN
160
Hardness x 10, GPa
140
120
100
80
60
40
20
0
0 200 400 600 800 1000 1200 1400 1600
Displacement Into Surface (nm)

Fig. 8: Load and hardness (x10) versus indenter penetration for a single test on a 200-nm gold coating on mica.
Discontinuities indicate fracture of the mica

(a)
100
90
80 Average of 8 CSM tests
10 ISO 14577 tests
70
Modulus (GPa)

60
50
40
30
20
10
0
0 200 400 600 800 1000 1200 1400 1600
Displacement Into Surface (nm)
(b)
10
9
8 Average of 8 CSM tests
10 ISO 14577 tests
7
Hardness (GPa)

6
5
4
3
2
1
0
0 200 400 600 800 1000 1200 1400 1600
Displacement Into Surface (nm)

Fig. 9: For a 200-nm gold coating on mica, (a) average modulus and (b) average hardness versus indenter
penetration depth. CSM values are averages of the data in Fig. 5. Error bars represent one standard deviation on
the average. Values obtained by testing according to ISO 14577 are also shown

May/June 2010 EXPERIMENTAL TECHNIQUES 93

CSM DURING INSTRUMENTED INDENTATION TESTING
not shown, because the oscillation caused the indenter to lose
contact with the sample. This is not an uncommon problem
for soft metals—the elastic recovery is so slight that the
excitation required for an oscillation as small as 2 nm can
cause the indenter to lose contact with the sample.12
The drops in hardness, most evident at about 1000 nm,
are due to fracture of the mica substrate. That fracture
is occurring is evident from the force-displacement curve
as shown in Fig. 8. The G200 Nanoindenter is electromag-
netically actuated, which means that it is fundamentally
force-controlled. As the applied force increases, the penetra-
tion depth also increases correspondingly. But at some point,
a small increase in force causes a significant jump in dis-
placement. Such behavior always indicates failure of some
sort.
Each CSM test returns Young’s modulus and hardness as a
function of indentation depth. The properties of the film alone
were calculated by averaging over a displacement range of
75–100 nm. For example, the value of film modulus for the
single test plotted in black in Fig. 7a (E1 ) was calculated
as the average of all readings between 75 and 100 nm. The
same procedure was repeated for every test to get E2 , E3 ,
and so on.
Finally, the average and standard deviation were calculated
for all n = 8 valid tests as
1
n
E= Ej , (31)
n 5. Loubet, J-L., Lucas, B.N., and Oliver, W.C., ‘‘Some Measure-
j =1
and
 tation and the Dynamic Characterization of Viscoelastic Solids,’’
1 n
σ (E) = 
2
(Ej − E) . (32)
n 7. Herbert, E.G., Oliver, W.C., Lumsdaine, A., and Pharr, G.M.,
j =1
A similar analysis was repeated for hardness. Using this
analysis, the measured properties for this gold film were:
• E = 69.8 ± 2.14 GPa
• H = 2.02 ± 0.19 GPa
To simplify the presentation of properties as a function
of penetration depth, channels of Young’s modulus and
hardness were also averaged into discrete displacement
windows. For this gold film, we chose a window size of 4 nm
and a systematic increase in window size of 5%. So, readings
from all tests for which displacement was between 0 and
4 nm were used to calculate average and standard deviation
for Young’s modulus and hardness for the first window.
Then, readings from all tests for which the penetration depth
was between 4 and 8.2 nm were used to calculate average
and standard deviation for Young’s modulus and hardness
for the second window. This same process was repeated until
the sliding and expanding window reached the maximum
94 EXPERIMENTAL TECHNIQUES May/June 2010
displacement. The black traces in Fig. 9 were generated in
this way.
CONCLUSIONS
CSM is a valuable tool for instrumented indentation testing.
CSM is often used to measure properties of thin films and
surface layers as a continuous function of penetration depth.
CSM should always be used when testing materials that
exhibit significant viscoelasticity or viscoplasticity (creep),
because for such materials, the semistatic force-removal
curve cannot be used to determine stiffness. If it is important
to measure properties according to a standard test method
such as ISO 14577 or ASTM E2546, then CSM can be used
for preliminary testing to determine the ideal peak force or
depth that should be used for the standard measurements.
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