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In this work, we investigated the bulk phase distinguishing of the poly(ε-caprolactone)-polybutadiene-poly(ε-caprolactone) (PCL-PB-PCL) triblock copolymer blended in epoxy resin by tapping mode atomic force microscopy (TM-AFM). We found that at a set-point amplitude ratio ( r  sp ) less than or equal to 0.85, a clear phase contrast could be obtained using a probe with a force constant of 40 N/m. When  r  sp  was decreased to 0.1 or less, the measured size of the PB-rich domain relatively shrank; however, the height images of the PB-rich domain would take reverse (translating from the original light to dark) at  r  sp  = 0.85. Force-probe measurements were carried out on the phase-separated regions by TM-AFM. According to the phase shift angle vs.  r  sp  curve, it could be concluded that the different force exerting on the epoxy matrix or on the PB-rich domain might result in the height and phase image reversion. Furthermore, the indentation depth vs.  r  sp  plot showed that with large tapping force (lower  r  sp ), the indentation depth for the PB-rich domain was nearly identical for the epoxy resin matrix.

The nanoscale phase distinguishing of PCL-PB-PCL blended in epoxy resin by tapping mode atomic force microscopy