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PolymersPolymers
  • Article
  • Open Access

15 May 2019

23 Pages

Visualization of Polymer Crystallization by In Situ Combination of Atomic Force Microscopy and Fast Scanning Calorimetry

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1
Institute of Physics and Competence Centre CALOR, University of Rostock, 18051 Rostock, Germany
2
Department of Polymer Science and Engineering, School of Chemistry and Chemical Engineering, Key Laboratory of High-Performance Polymer Materials and Technology of Ministry of Education, and The State Key Laboratory of Coordination Chemistry, Nanjing University, Nanjing 210093, China
3
Shenyang Research Institute, Nanjing University, Shenyang 224300, China
4
Interdisciplinary Center for Transfer-oriented Research in Natural Sciences (IWE TFN), Martin Luther University Halle-Wittenberg, 06099 Halle/Saale, Germany

Abstract

A chip-based fast scanning calorimeter (FSC) is used as a fast hot-stage in an atomic force microscope (AFM). This way, the morphology of materials with a resolution from micrometers to nanometers after fast thermal treatments becomes accessible. An FSC can treat the sample isothermally or at heating and cooling rates up to 1 MK/s. The short response time of the FSC in the order of milliseconds enables rapid changes from scanning to isothermal modes and vice versa. Additionally, FSC provides crystallization/melting curves of the sample just imaged by AFM. We describe a combined AFM-FSC device, where the AFM sample holder is replaced by the FSC chip-sensor. The sample can be repeatedly annealed at pre-defined temperatures and times and the AFM images can be taken from exactly the same spot of the sample. The AFM-FSC combination is used for the investigation of crystallization of polyamide 66 (PA 66), poly(ether ether ketone) (PEEK), poly(butylene terephthalate) (PBT) and poly(ε-caprolactone) (PCL).

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