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Jan. 23, 2012

Fig. 1: Interface between EPON resin (gray mark) and PEMMA polymer (red mark). Image is acquired ... more

A simple method to direct identify nanometer sized textures in composite materials by means of **AFM Spectroscopy**, aiming at recognizing nanometer structures embedded in a sample. It consists in acquiring a set of dynamic data organized in spectroscopy maps and subsequently extracting most valuable information by means of the **Principal Component Analysis** (PCA) method [1]. In this work we explain the main features of the method and show its application on a nanocomposite sample.

**Force Spectroscopy by AFM**

Local properties of materials with nanometer resolution can be probed by means of atomic force microscope, performing force spectroscopy experiments: in these experiments, tip-sample interaction forces are measured acquiring quasi-static cantilever deflection as a function of separation while the tip is brought into contact with the sample and then far apart from it.

Force-distance (FD) curves contain valuable information about nanoscale material properties [2] such as adhesion, elasticity and plasticity, as well as friction. Several mathematical models have been proposed and used to model the different ideal situations of tip sample interaction, where rounded tips with well known curvature radius interact with a flat surface-hypothesis is not always verified-in presence (JKR and DMT) or in absence (Hertz) of adhesion.

An accurate evaluation of each FD curve of a 3D spectroscopy map (2D arrays of FD curves) is, in most cases, time consuming, especially in biological samples that use a more refined model. If we shift to dynamic AFM, in which the cantilever is dithered close to its resonance frequency, we can use the same approach with the so called "dynamic force spectroscopy" but the complexity of the system is considerably raised. In this case we will collect several parameters as a function of distance (such as static deflection, amplitude, phase, higher harmonics frequency shifts, etc.) containing a larger amount of data. As shown by several authors [3,4], approach curves contain valuable information about chemical composition, short and long range interaction forces, friction and plasticity.

In relation to what has been told introducing secondary oscillations (multifrequency AFM) during imaging has shown interesting results in enhancing material contrast going "beneath the surface" but the theoretical understanding is still under development [5].

**Applying PCA to Data**

The huge amount of information requires a higher computational weight to reconstruct physically valuable parameters in comparison with contact models; as a result a fast and easy analysis relying on these dynamic methods is still far to be routinely implemented to spectroscopy maps or it is limited to few information.

Principal Component Analysis (PCA) method [6] has been successfully applied to compress complex data series and is the right statistical tool to facilitate the analysis of multi parameters maps [7,8].

In short, this algorithm projects the information of D (e.g. amplitude, phase, freq. etc.) spectroscopy curves, each containing P values (depending on sampling frequency), acquired at each point of an L x C grid into a subset of L x C maps without any assumption on the sample structure, filtering out redundancies and noise. As a consequence, a huge amount of 3D data is condensed into few 2D maps, easy to be examined.

Data from all channels is grouped together and analyzed: in this way data is reduced to maps with L x C dimensionality, summing up independent information from each parameter and from all of them. This process is intended to find different features within the probed region (in the following example a 5 x 5 µm^{2} interface area) and to evaluate, at the same time, the response on different dynamic parameters: results therefore provide a robust and quick screening method to locate region of interest (ROI) on the sample, where further investigations can be addressed.

**Example of Application**

The area is shown in figure 1; the selected area is imaged in amplitude modulation. The sample considered is the interface region between EPON resin (left) and PEMMA polymer (right).

The following step is the acquisition of the approach curves. The area is divided into a 64 x 64 grid, we obtain for each point 4 vectors corresponding to the 4 channels acquired: Amplitude (variation of amplitude oscillation of the main vibration mode, used also as trigger channel; Amplitude2 (variation in amplitude of a secondary oscillation, in this case the second harmonic); Phase; Frequency (shifts in frequency of primary "driven" oscillation) All sampled at 2.147 Hz. On the right column we can see the spectroscopy data for two points (1, 2). The plastic behavior, recognizable from the differences between traces and retrace in channel (e) and (f), is expected; it is noticeable to see the high sensitivity of frequency and second harmonic channel in comparison to the amplitude signal. It is also interesting to notice how channel (f) for instance exhausts its main contribution 50 nm above the Amplitude trigger point in position 2, while same channel in position 1 still have high sensitivity. Given the input vectors, PCA is applied. We retained a number of components sufficient to explain a given amount of variance (98 %). In figure 2 the results are shown: the Region Of Interest (ROI) we focused our attention on is at the interface between polymer and resin. The two areas have different composition and, in a narrower scale, different roughness and different mechanical properties. The first principal component on each spectroscopy channel is shown: maps (a), (b), (c), and (d) show results on amplitude, second harmonic, phase and frequency. Figure 4e is the first component of PCA on data from all components.

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**Keywords**: compositional contrast Dynamic Force Spectroscopy Material Sciences Multifrequency AFM Nanotechnology PCA Principal Component Analysis Region Of Interest

**Italian Institute of Technology**

Nanophysics Department

Genova

Italy

Web: http://www.iit.it

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