How To Choose   AFM Experiment  

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.

(a)(b)
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.

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.

However, it is still challenging to distinguish between the different properties of materials like stiffness, hardness, adhesion, and viscoelasticity on these compositional maps.

 

Lateral force microscopy

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.

(a)(b)
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.

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

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 DP18 series which features an intermediate spring constant of ~5 N/m.

Resolution of the scans depends on the type of the probe tip.

 

Phase imaging

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 DP14 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.

LFM


High lateral resolution
GP probes for contact mode
DP17/GP/ALBS


Higher sensitivity to lateral forces
LS probes with large tip radius
DP19/LS/ALBS

force modulation


Unknown sample
GP probes with medium spring constant DP18/GP/AlBS


Soft sample
GP probes with low spring constant
DP17/GP/ALBS


Hard sample
GP probes with high spring constant
DP16/GP/ALBS

Phase imaging


Unknown sample
GP probes with a medium spring constant DP14/GP/AlBS


High resolution imaging
Hi'RES probe
DP14/Hi-RES-W/AlBS


Soft sample
Hi'RES probe mounted on soft cantilever
DP19/Hi'RES-C/AlBS


Hard sample or imaging of
sub-surface structures

GP probes with high spring constant
DP15/GP/AlBS

 
 

 

 

 

 
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