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Open Access Nano Express

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

Huiqin Li1, Limin Sun1, Guangxia Shen2 and Qi Liang1*

Author Affiliations

1 Instrumental Analysis Center, Shanghai Jiao Tong University, Shanghai, 200240, China

2 Research Institute of Micro/Nano Science and Technology, Shanghai Jiao Tong University, Shanghai, 200240, China

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Nanoscale Research Letters 2012, 7:153  doi:10.1186/1556-276X-7-153

Published: 23 February 2012

Abstract

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 (rsp) 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 rsp 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 rsp = 0.85. Force-probe measurements were carried out on the phase-separated regions by TM-AFM. According to the phase shift angle vs. rsp 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. rsp plot showed that with large tapping force (lower rsp), the indentation depth for the PB-rich domain was nearly identical for the epoxy resin matrix.

Keywords:
tapping mode AFM; PCL-PB-PCL; phase image; force-probe