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

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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… Click to show full 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).

Keywords: combination; microscopy; fast scanning; crystallization; atomic force

Journal Title: Polymers
Year Published: 2019

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