Material Composition
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In addition to the surface topography, AFM allows probing different
mechanical properties of materials. This type of experiment can
be utilized to enhance imaging contrast of topography scans and
to map the materials of heterogeneous samples.
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| Fig.1. Height (a) and phase (b) images
of biaxially oriented high density polyethylene film obtained in the
tapping mode. Scan size 400 nm. Images are courtesy of S. Magonov. |
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Compositional mapping of mechanical properties can be conducted
in Contact and Tapping mode. In Contact mode, one usually employs
two imaging modes: Lateral Force Microscopy (LFM) to probe local
friction and Force modulation to map material elasticity. Phase
imaging is one of the imaging modes of Tapping mode AFM, which is
sensitive to local viscoelasticity, adhesion, and friction properties
of a sample.
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However, it is still challenging to distinguish between the different
properties of materials like stiffness, hardness, adhesion, and
viscoelasticity on these compositional maps.
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Lateral force microscopy
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Lateral Force Microscopy (LFM), in which lateral force images are
detected, is more sensitive to variations of stiffness and adhesion
in heterogeneous samples, for example, in organic layers prepared
from a mixture of components. For LFM measurements one can use the
probes with the same stiffness as those applied in the contact mode
studies. However, the cantilever geometry can be optimized to get
larger lateral force sensitivity, as in the novel NanoTwist probes
with the tip position offset from the main cantilever axis.
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| Fig.2. Gold evaporated on mica with organic
layer. Gold islands reveal lower friction. Trace (a) and retrace (b)
images, left to right and right to left.Scan size 1 µm.
Image courtesy of L.V. Kulikova and I.V. Yaminsky, MSU&ATC. |
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LFM images of gold evaporated on mica with organic layer are presented
in Fig. 2. One might note the tip artefact resulting in similar
outline of all the surface features, especially the smallest. This
tip artefact might be probably caused by the tip damage due to high
loads exerted in LFM.
For this reason, LFM may require LS tips because they present a
larger tip-sample interaction area producing a stronger lateral
deflection of the cantilever. The larger cantilever deflection must
be balanced against the lower lateral resolution delivered by the
blunter tip.
Force modulation and contact resonance
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There are two other techniques: Force Modulation (FM) and Contact
Resonance (CR), which are aimed on studies of local mechanical properties
with the AFM probe staying in a permanent contact with a sample.
They are actually oscillatory methods in which a tip or a sample
is driven into an oscillation by a piezoelement or a broadband transducer.
In FM the cantilever is forced to oscillate at the resonant frequency
of the piezoelement (typically ~5-10 kHz) and the deflections of
the cantilever are measured at the same frequency. This deflection
(or its amplitude) will be large when the tip hits a stiffer location
and the related contrast in the FM Amplitude image provides a compositional
map of the sample. Typically, Si probes with stiffness between 0.5
N/m and 5 N/m are applied for this purpose.
In the CR technique, the information is gained from the frequency
spectrum of the probe staying in contact with a sample. The shifts
of the resonant probe frequency and phase due to mechanical interactions
with the sample are measured and applied for an estimation of its
mechanical properties. Si probes with stiffness from 0.1 N/m to
5 N/m might be used in these experiments. From viewpoint of quantitative
mechanical measurements, it can be attractive to use the probes
with tips that have larger apex with well-defined dimensions.
To get a high-contrast image in Force Modulation, cantilever and
sample should be matched in terms of stiffness. Different cantilevers
can be used to find the best match. For samples with unknown mechanical
properties, it is recommended using a probe of the 18 series which
features an intermediate spring constant of ~5 N/m.
Resolution of the scans depends on the type of the probe tip.
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Phase imaging
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The development of phase imaging was another pivotal event that
made AFM a recognized characterization technique especially for
examination of heterogeneous materials. The difference between phase
of free-oscillating probe (or phase of the oscillating piezoelectric
transducer that drives the probe) and the phase of the probe oscillation
while it interacts with a sample appeared to be very sensitive to
variations of mechanical, adhesive and electromagnetic properties.
The contrast of the phase images of multicomponent materials reveals
a distribution of individual components. Imaging at elevated forces
with probes whose stiffness is close to that of the components is
particularly important for getting high-contrast phase images. The
fact that contemporary materials include components with very broad
spectrum of mechanical properties means that the optimization of
imaging conditions requires a proper selection of the probe stiffness.
For successful imaging of soft samples such as polymers or biomaterials,
the cantilever spring constant should match the effective spring
constant of the tip-surface contact area. For samples with unknown
mechanical properties, it is recommended using a probe of the 14
which features an intermediate spring constant of ~5 N/m.
"Hard" tapping (larger amplitudes and low set point ratios)
is usually required to achieve strong material-sensitive contrast
in phase image.
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