Abstract

A key application of atomic force microscopy (AFM) is the measurement of physical properties at sub-micrometer resolution. Methods such as force–distance curves (FDCs) or dynamic variants (such as intermodulation AFM (ImAFM)) are able to measure mechanical properties (such as the local stiffness, kr) of nanoscopic heterogeneous materials. For a complete structure–property correlation, these mechanical measurements are considered to lack the ability to identify the chemical structure of the materials. In this study, the measured attractive force, Fattr, acting between the AFM tip and the sample is shown to be an independent measurement for the local chemical composition and hence a complete structure–property correlation can be obtained. A proof of concept is provided by two model samples comprised of (1) epoxy/polycarbonate and (2) epoxy/boehmite. The preparation of the model samples allowed for the assignment of material phases based on AFM topography. Additional chemical characterization on the nanoscale is performed by an AFM/infrared-spectroscopy hybrid method. Mechanical properties (kr) and attractive forces (Fattr) are calculated and a structure–property correlation is obtained by a manual principle component analysis (mPCA) from a kr/Fattr diagram. A third sample comprised of (3) epoxy/polycarbonate/boehmite is measured by ImAFM. The measurement of a 2 × 2 µm cross section yields 128 × 128 force curves which are successfully evaluated by a kr/Fattr diagram and the nanoscopic heterogeneity of the sample is determined.

Highlights

  • The mechanical properties of small volumes of materials can be measured using various atomic force microscopy (AFM) methods

  • 50 force–distance curves (FDCs) per material were evaluated for their parameter sets kr and Fattr, as shown in Figure 2a and Figure 2b

  • By taking advantage of this statistical approach, we showed that the maximum attractive force Fattr of any given force curve strongly depends on the chemical species present in the measured volume

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Summary

Introduction

The mechanical properties of small volumes of materials can be measured using various atomic force microscopy (AFM) methods. Method is the most fundamental force spectroscopy experimental setup which yields local mechanical properties with a lateral resolution between 500 nm and 1 μm [1,2,3]. Ments have aimed to increase the lateral resolution of force spectroscopy by implementing dynamic methods. This has resulted in methods such as force modulation [4], bimodal mode [5], pulsed-force mode [6] or peak force [7], and intermodulation AFM (ImAFM) with amplitude-dependent force spectroscopy (ADFS) [8,9,10]. Dynamic methods record local mechanical properties with a resolution in the range of the tip radius R of the AFM probe (typically 4 nm ≤ R ≤ 40 nm)

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