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Rapid Mechanical Properties of
Multi-layer Film Stacks

Application Note

Jennifer Hay,
Agilent Technologies




Abstract                                      Agilent's most recent leap in technology,
In this work, we measure the mechanical       Express Test, improves our ability to
properties of 50nm films with remarkable      characterize thin films by dramatically
precision and accuracy. The precision         increasing the number of independent
is due to Express Test, which performs        measurements which can be made in a
indentations at a rate of one per second,     given time period. Why is it important to
thereby allowing many indentations to         make more measurements on thin films?
be included in the final determination        It is important, because nanoindentation
of modulus and hardness. The accuracy         measurements of Young's modulus and
is due, in part, to an analytic model         hardness tend to grow more scattered
which yields the substrate-independent        as the indentation depth decreases,
moduli of thin films. In order to apply the   primarily due to surface roughness,
thin-film model to a stack of multiple        but more scatter can be overcome with
films, the film modulus of each new           more measurements. Express Test
layer is determined and then used as          is Agilent's proprietary technology
the "substrate" modulus for the next          for rapid indentation. Express Test
layer. This process could be repeated         performs indentations in less than five
ad infinitum. The thin-film model reveals     seconds, thus dramatically increasing
a large difference in Young's modulus         the number of statistically independent
between two 50nm films.                       measurements which can be made in a
                                              given time period.

Introduction                                  For all its advantages, Express Test is
The primary motivation behind                 nanoindentation at its simplest. The
nanoindentation has always been the           indenter approaches the test surface
desire to measure the mechanical              until contact is detected, loads to
properties of small volumes of material,      achieve the target force or displacement,
especially in the form of thin films. In      withdraws the indenter from the
the present application, we see how two       sample, and then moves the sample into
recent developments in nanoindentation        position for the next indentation. The
work together to allow the quantitative       contact stiffness is calculated using
characterization of films as thin as 50nm.    the upper 50% of the unloading curve
                                              (i.e. forces which are greater than 50%
of the peak force, and corresponding                    properties of the supporting substrate.            Experimental Method
displacements, acquired during                          However, Agilent's proprietary thin-               Samples
unloading). All downstream calculations                 film model fully accounts for substrate            The samples identified in Table 1
such as contact depth, contact area,                    influence, regardless of whether the               were tested. Basically, the substrate
hardness and Young's modulus are                        film is stiffer or more compliant than             was tested alone (sample 1) and then
calculated according to established                     the substrate. The details of this model           subsequent layers were tested as they
norms, and Young's moduli measured by                   are provided elsewhere, and are not                were deposited.
Express Test agree with values measured                 reiterated here [4, 5].
by other means for a wide variety of                                                                       Equipment and Procedure
materials. Express Test derives its speed               In the present application, we show                All samples were tested with an Agilent
not from novel procedures or analyses,                  how these two advances, Express                    G200 NanoIndenter, configured with
but from a comprehensive understanding                  Test and thin-film modeling, combine               the Express Test option. All tests were
of instrument dynamics, combined with                   to dramatically improve thin-film                  performed using a DCM II head fitted
strategic advances in data acquisition                  characterization. Figure 1 shows a                 with a Berkovich indenter. Sample
and storage [1].                                        schematic of the unique material tested            positioning was accomplished with the
                                                        in this work. The substrate is a sintered          NanoVision option. This combination of
Like other indentation methods,                         composite of alumina (Al2O 3) and                  hardware (the DCM II and NanoVision
Express Test returns a triplet of force,                titanium carbide (TiC), the microstructure         stage) allowed Express Test to perform
displacement, and stiffness for each                    of which is shown in Figure 2. Upon this           one indentation every second.
indentation, but this information is only               substrate is a layer of sputter-deposited
as good as the model which relates these                Al2O 3 having a thickness of 2600nm. The           Preliminary testing was done on
fundamental measurements to useful                      topmost layer of this structure is 50nm            sample 2 in order to know the depth
mechanical properties, such as Young's                  of either silica (SiO 2) or alumina (Al2O 3).      profile of properties for this material.
modulus and hardness. The most basic,                   The properties of each layer are not only          This preliminary test was accomplished
and oft-cited, model for interpreting                   important in their own right, but also             with the method "Express Test, Varied
fundamental indentation measurements                    must be known in order to accurately               Force" which automatically performs
is due to Ian Sneddon, but Sneddon's                    calculate the properties of subsequent             an array of 20 x 20 indentations over
model presumes that the test material                   layers via the thin-film model. Thus,              an appropriate range of forces within a
is large and uniform throughout [2, 3].                 in this work, we provide a practical               100 

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