Micro- and Nano-scale Measurement of the Thermophysical Properties of Polymeric Materials Using Atomic Force Microscopy

To realize the benefits and optimize the performance of micro- and nano-structured materials and thin films, designers need to understand and thus be able to characterize their thermal, thermophysical, and thermomechanical properties on appropriate length scales. This paper describes the determination of glass-transition temperatures of polymers on the micro-scale, obtained from contact force–distance curves for poly(methyl methacrylate) and poly(vinyl acetate) measured using an atomic force microscope (AFM). Measurements were made using a standard AFM tip where thin films were heated using a temperature controlled hot stage and by using a scanning thermal microscopy (SThM) probe. The latter was used either with the hot stage or with the SThM probe providing a localized heating source via Joule heating. Differences in the glass-transition temperature measured using the hot stage and Joule heating were apparent and considered to be due to heat transfer effects between the probe, specimen, and surroundings. Gradients of force–distance curves, pull-off and snap-in forces, and adhesion energy were obtained. The results suggest that the onset of changes in the material’s mechanical properties at the glass transition was found to be dependent on the mechanical property measured, with pull-off force values changing at lower temperatures than the snap-in force and adhesion energy.