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Application Note

Depth-dependent measurements with the QCSM module


01 Description of testing situations and their

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ranges of application

Conventional indentation hardness


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Nanoindentation with ZHN The contact depth hc is determined with the help of a
model from the maximum depth and the contact stiff‐
During depth sensing nanoindentation measurements ness S at maximum load. This corresponds to the slope
for the determination if the indentation hardness HIT of the tangent to the unloading curve (blue line). There‐
according to DIN EN ISO 14577, the load-displacement fore, indentation hardness and modulus can only be
curve F(h) is measured with a certain maximum load. determined if the contact stiffness is measured.
The hardness can only be given for the maximum depth
which is reached in this measurement. A hardness
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profile along the depth can only be determined by many


measurements with different loads on different places of
the sample. This is a time-consuming procedure and
requires much effort for the analysis of the data.
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With the CSM or QCSM method, the contact stiffness is


measured already during loading as quotient of force
amplitude and displacement amplitude of a small oscil‐
lation.

For the calculation of hardness H and reduced modulus


Er the contact area Ac is used. It can only be obtained
from the contact depth hc.
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Application Note
Depth-dependent measurements with the QCSM module
Comparison of CSM and QCSM switched on during a short dwell time between about
0.5 s and 3 s (see principle of QCSM method). This
The Continuous Stiffness Measurement (CSM) method allows an easy averaging of several oscillations and also
adds a continuous small oscillation to the force signal. the feedback control is more accurate. For example
The ratio of force and displacement amplitude delivers there are amplitudes from 56 oscillations measured at a
the contact stiffness between indenter and sample after frequency of 40 Hz and a dwell time of 1.4 s. In the
some corrections which consider moving mass, QCSM method the first 20 % of the measured
frequency and damping coefficient. In the CSM method amplitudes are not considered for averaging to reduce
the static force during loading is for every oscillation the creep influence on the results. This is especially
slightly different. This complicates the averaging of important for viscous materials.
several oscillations and the feedback control.
In contrast during the QCSM method the force is
increased in small steps and the oscillation is only
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Principle of CSM method Principle of QCSM method

Figure 3 shows an example. There are all measured


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amplitudes visible during a 1.4 s dwell time in one force


step of a Berkovich indentation into sapphire. The
displacement amplitude was chosen small do
demonstrate the resolution and to disturb the
measurement as less as possible. For a comparison
with other instruments it has to be considered that the
maximum amplitude is given in the ZHN software and
not the root mean square value. The following results
are obtained:
• Displacement amplitude: 2.46 nm; standard deviation
0.22 nm; statistical error 2.8 %
• Force amplitude 0.741 mN; standard deviation 0.0025
mN; statistical error 0.1 %
The accuracy can further be improved by a longer dwell Amplitudes of all single oscillations during a dwell time of 1.4 s and for
time or larger amplitude. a frequency of 40 Hz. The first 12 of 56 oscillations are not used for
averaging because creep effects are largest immediately after
reaching the target force.

All data at ambient temperature. We reserve the right to make technical changes in the course of ongoing
development.
Application Note
Depth-dependent measurements with the QCSM module
The CSM as well as the QCSM method allow a depth-

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resolved measurement of hardness and modulus at one
and the same position. Therefore much more
information can be generated than with normal
indentation measurements. The default value for the
force step number in a QCSM application is 30. This
corresponds to measurements with 30 different forces.
Further the accuracy of QCSM measurements is higher
at very small forces. With the 2 N measuring had it is
therefore possible to measure accurate data at only 100
µN or 10 nm depth.
The results of the QCSM method are independent on
the frequency up to about 75 Hz (in dependence on
material and indenter shape). This is demonstrated in
fig. 4 for fused silica measurements. The curves for the Detail from figure 4 as comparison of CSM and QCSM measurements
depth-dependent modulus have been obtained by with the same frequency of 40 Hz. These are average curves from 6
averaging 6 single measurements. The error bars show single measurements. Error bars give the statistical error. The smaller
error for the QCSM method can be recognized.
the statistical error. A more resolved comparison
between CSM und QCSM method in fig. 5 shows that A separate application allows a frequency sweep for the
the error of the CSM is clearly larger for the same determination of the frequency dependent e-modulus of
frequency of 40 Hz. viscous materials. Fig. 6 demonstrates this for the
measurement of an elastomer with the name Affinity. In
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this case correct measurements up to 100 Hz have


been possible by using a big ball of 7 mm diameter as
indenter. DMA data up to 20 Hz have been available for
the same sample so that a comparison was possible.
Considering the different contact geometry in an
indentation experiment and a DMA test the results
agree very well.
Another speciality of the ZHN is that quite big force
amplitudes of 50 mN or more can be generated during
oscillations. This allows fatigue tests even with higher
frequencies than 75 Hz because no contact stiffness
needs to be calculated.
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Comparison of depth dependent modulus curves from CSM and


QCSM measurements on fused silica with different frequencies. For
the CSM measurement the acquisition rate was 8 Hz and the
oscillation frequency was 40 Hz.

Frequency dependent modulus of an elastomer in a frequency range


from 0.1 Hz to 100 Hz and comparison to the results of a DMA test
with the same sample (only up to 20 Hz)

All data at ambient temperature. We reserve the right to make technical changes in the course of ongoing
development.
Application Note
Depth-dependent measurements with the QCSM module
Abb. 7 zeigt eine Schwingung des Indenters gegen Luft
mit einer Frequenz von 10 Hz und einer Abtastrate von
512 Hz mit der Oscilloscope Funktion der
Gerätesoftware. Es werden immer 512 Punkte im Bild
dargestellt. Da die Werte durchlaufend erneuert werden,
ist immer an einer Stelle der Grafik ein Sprung zu
erkennen (hier bei 0,9 s), der jedoch keine
Beeinträchtigung der Funktion darstellt.
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Oscilloscope function for an oscillation in air with 10 Hz and an


acquisition rate of 512 Hz.

Figure 8 shows the complete oscilloscope window with


the maximum oscillation frequency of 300 Hz also for
oscillations in air. The acquisition rate was 13 kHz here.
The maximum acquisition rate of the ZHN is 40 kHz.
Due to the inert mass of the oscillating parts the system
cannot follow quickly enough so that the force signal
becomes significantly larger than the displacement
signal. After contact with a stiff sample the amplitude
ratio will change. This example demonstrates nicely the
independency between force measurement and force
generation for the ZHN head. The indenter can oscillate
freely and is not damped by the actor (piezo element).
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Oscilloscope window for an oscillation in air with 300 Hz and an


acquisition rate of 13 kHz. The inert mass of the moving parts result in
a significantly larger force signal than displacement signal.

All data at ambient temperature. We reserve the right to make technical changes in the course of ongoing
development.
Application Note
Depth-dependent measurements with the QCSM module
02 Solutions available from the ZwickRoell

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Group
The Universal Nanomechanical Tester is designed for
the determination of hardness and Young's Modulus on
materials and coating systems. The nano and micro
ranges are compliant to the standard EN ISO 14577
(instrumented indentation method for determining
hardness and other material parameters of metallic
materials and coatings). The Nanonmechanical Tester
can also perform cyclic indentation tests and
indentation tests with superimposed oscillation.
Due to its high level of modularity it is more than a
nanoindenter or hardness tester. It can be used with a The ZHN nanoindenter
measuring head (NFU) as a:
Advantages and features
• Nanoindenter / hardness tester for measurements • Modern software, with clearly structured design
between 0.05 mN - 20000 mN depending on the • Stiff frame design with indenter axis exactly in the
measuring head used movement axis (no tilting moment)
• Micro tensile testing instrument in the same force • High degree of modularity provided by:
range ‒ interchangeable measuring heads in normal (20 N /
• Fatigue tester up to 2 Hz quasi-static or up to 300 Hz 2 N / 0.2 N) and lateral directions, allowing realistic
with dynamic module modeling of loading conditions
• Dynamic mechanical tester (DMA) up to approx ‒ unique tandem optics (developed for space travel)
100 Hz with dynamic module with 2 cameras; can be expanded for up to 4
• Profilometer and with dynamic module also stiffness/ different magnifications
modulus mapping ‒ software structure features function / application
• Scratch tests modules for hardness and Young's modulus tests,
With a second measuring head for lateral force scratch test, cyclic indentation test and indentation
displacement curve (LFU) it can be used as: test with superimposed oscillation
• Various specimen holders available, including holders
• Scratch test with measurement of the frictional force
with insulated specimen carriers for tip – specimen
• Oscillating scratch test (oscillation of the specimen
contact resistance measurement
vertically in the scratch direction)
• Ample room in all directions, with precise step size
• Micro wear tester for reversing wear
and high resolution:
• Micro fretting tester (lateral oscillation) with dynamic
‒ X-direction: 100 mm
module
‒ Y-direction: 200 mm
• Measuring device for elastic lateral deformations The
‒ Z-direction: 70 mm
following can be derived:
• New enclosure design with improved thermal and
‒ Lateral contact stiffness
acoustic insulation
‒ Poisson's ratio
‒ Lateral failure mechanisms
NOTE
This Application Note has been produced to
the best of our technical knowledge and with
all due care. It is nevertheless possible that, for
material or application-related reasons, test
results may have to be obtained using altered
methods In this regard our Application Notes
are guidelines to performing tests.

All data at ambient temperature. We reserve the right to make technical changes in the course of ongoing
development.

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