高速差示扫描量热分析技术在聚合物材料上的应用.ppt

Applications of HyperDSC on Polymeric Materials高速差示扫描量热分析技术在聚合物材料上的应用 Differential Scanning Calorimetry Glass Transition Temp. (Tg) Onset Temperatures Melting Points (Tm) Crystallinity Heats of Fusion Purity Rates of Reaction Curing Specific Heat Heat Capacity Oxidative Stability Crystallization What is HyperDSC?? A New Technique for Material Characterisation An additional/alternative technique to DSC providing extra sample information Information collected in Seconds Why Increased sensitivity? Sensor Temperatures at various rates Indium Before Calibration - Nitrogen Purge Indium Before Calibration - Nitrogen Purge Thermal lag surprisingly small Near linear energy performance 10% variation at 500oC/min These taken account of by calibration Indium after Calibration Small Transients at the start allow data to be obtained without going to extremely low temperatures Hyper DSC? Applications Fast identification of polymeric materials PP granule (quick cooled) Polyamide 10:6 Heating at 10, 100, 200°C/min Example of different crystallization behaviour at high cooling rates compared to cooling at 10°C/min The big difference in melting temperature at 150°C is related to the crystal structure. At 10 C/min reorganization is giving a false picture of the mechanical properties at room temperature Food Packaging Film Polypropylene Tg at low scan rate Polypropylene Tg of BMI Composite Tg of BMI Composite Use of HyperDSC? in the Identification of the Glass Transition of Nifedipine Case Study: Measure Tg of epoxy Summary: A challenge in the characterization of epoxy cure with DSC is the overlap between the glass transition and the curing exothermal. Since the glass transition is independent of rate, whereas the curing reaction is dependent, scanning rate can be used to shift the exothermal while not affecting the glass transition temperature. At 100°C/min, the two overlapping events are separated,