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).
Highlights
With the opportunity to cool and heat samples at extremely high rates, fast scanning chip calorimetry (FSC) has become an invaluable tool in materials research
The atomic force microscope (AFM)-fast scanning calorimeter (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)
Even though the anticipated results were not obtained, we present this example to highlight specific observations of in situ AFM during crystallization and, show how fast scanning calorimetry in combination with AFM can overcome these limitations in an elegant and advantageous way
Summary
With the opportunity to cool and heat samples at extremely high rates, fast scanning chip calorimetry (FSC) has become an invaluable tool in materials research. Chan’s group [28,31,32] used an AFM hot-stage combination to successfully follow the process of polymer crystallization in real time, starting from the unstructured melt, following the formation of lamellae and the growth of spherulites. They showed how homogeneous and heterogeneous nucleation influence the crystallization process.
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