In Situ Nanostress Visualization Method to Reveal the Micromechanical Mechanism of Nanocomposites by Atomic Force Microscopy.

An in situ atomic force microscopy (AFM) nanomechanical technique was used to directly visualize the micromechanical behaviors of polymer nanocomposites during compressive strain. We obtained a stress distribution image of carbon black (CB)-filled rubber at the nanoscale for the first time, and we traced the microscopic deformation behaviors of CB particles. Through this experiment, we directly revealed the microscopic reinforcement mechanisms of rubber composites. We found that CB-filled rubbers exhibited heterogeneous local microscopic deformations, which were related to the dispersion of CB particles in rubber matrices. The local stress distributions of the rubber composites showed heterogeneity, and the stresses were concentrated in the regions near the CB particles during compression. The area of stress concentration gradually expanded with increasing strain and eventually formed a stress network structure. This stress network bore most of the macroscopic stress and was considered the key reinforcement mechanism of CB-filled rubber. The stress transfer process in the rubber matrix was visualized in real space for the first time. Based on the image data from the AFM experiments, we used finite-element method (FEM) simulations to reproduce the microscopic deformation process of CB-filled rubber. The stress distribution images simulated by FEM showed heterogeneity consistent with AFM. In this study, an in situ visualization of material deformation confirmed the predictions of microscopic deformation behavior from previous theories and models; it also provided new insights into the microscopic reinforcement mechanisms of CB-filled rubber composites based on microscopic stress distribution images.