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Updated: Oct 8, 2025

Atomic Force Microscopy Cantilever-Based Nanoindentation: Mechanical Property Measurements at the Nanoscale in Air and Fluid
Published on: December 2, 2022
Direct Visualization of Interfacial Regions between Fillers and Matrix in Rubber Composites Observed by Atomic Force
Makiko Ito1, Haonan Liu1, Akemi Kumagai2
1Department of Chemical Science and Engineering, Tokyo Institute of Technology, 2-12-1, O-Okayama, Meguro-ku, Tokyo 152-8552, Japan.
Abstract:
In order to explain or predict the macroscopic mechanical properties of polymer composites with complex nanostructures, atomic force microscopy (AFM)-based nanomechanics is one of the most appropriate tools because the local mechanical properties can be obtained by it. However, automatic force curve analysis based on contact mechanics would mislead us to the wrong conclusion. The purpose of this study is to elucidate this point by applying AFM nanomechanics on a carbon black (CB)-reinforced isoprene rubber (IR). The CB aggregates underneath the rubber surface prevent us from quantitatively evaluating the ratio of CB and interfacial polymer region (IPR), which is an important parameter to determine the macroscopic mechanical properties. In order to overcome this problem, transmission electron microtomography was incorporated to investigate the 3D structure in the same field of view as AFM nanomechanics. As a result, it was found that there are buried structures that do not appear in the AFM topographic image. In addition, we were able to reveal the existence of a force curve with an inflection point, which is characteristic of such "false" IPRs. To put it another way, we evidenced the existence of true IPRs for the first time by combining these state-of-the-art techniques.

