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Fast Scanning Chip Calorimetry
Fast scanning chip calorimetry (flash DSC) is a complementary technique to conventional differential scanning calorimetry (DSC) that allows for rapid and precise thermal analysis of materials. It offers ultra-high heating and cooling rates, enabling exploration of reorganization processes and structural formation in various materials. The flash DSC enhances manufacturing efficiency and product quality by providing critical insights into material behaviors under production conditions.
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Fast Scanning Chip Calorimetry
- 1. Fast Scanning Chip Calorimetry JürgenSchawe, PhD Senior Scientist, Thermal Analysis Mettler Toledo
- 2. An expert presentsan overview of why fast scanning chip calorimetry is the ideal complement to conventional DSC Fast Scanning Chip Calorimetry
- 3. Flash DSC Advanced MaterialsCharacterization by Fast Scanning Calorimetry Jürgen Schawe MSG MatChar August 2019
- 4. 4 Contents ▪ The DSCTechnique - Conventional DSC Curve of PET - Reorganization During the Measurement ▪ The Flash DSC - The Chip Sensor ▪ Metastable Materials ▪ Flash DSC Basics - Variation of Scanning Rates - Flash DSC Application Areas ▪ Application Examples ▪ Summary ▪ More Information
- 5. 5 The DSC Technique ConventionalDSC Measuring Principle Reference Sample Heat flow Typical experimental conditions: Sample weight: 1 … 20 mg Heating rate: 0.1 … 100 K/min Measured property: Heat flow
- 6. The DSC Technique:DSC Curve of PET 6 0
- 7. Reorganization During theMeasurement 7 0
- 8. Flash DSC (FDSC) FlashDSC ▪ Sensor UFS: −95 °C to 520 °C ▪ Typical heating rates: 0.1 to 20,000 K/s ▪ Typical cooling rates: 0.1 to 4,000 K/s ▪ Sensor UFH: −95 °C to 1000 °C ▪ Typical heating rates: 0.1 to 60,000 K/s ▪ Typical cooling rates: 0.1 to 40,000 K/s 8 Together, conventional DSC and Flash DSC cover a scanning rate range of more than 8 decades. 0.1 K/min 10 K/min 200 K/min 3 000 000 K/min
- 9. FDSC: Ergonomic Design 9 Easysample preparation and sensor change thanks to the Flash DSC's ergonomic design.
- 10. FDSC Chip SensorPrinciple 10 Ceramic plate Silicon frame Bonding wire Thermocouple Resistance heater Metal plate Standard UFS MultiSTAR sensor Standard UFS MultiSTAR sensor: close up The MultiSTAR UFS is a DSC chip sensor based on MEMS (Micro-Electro-Mechanical Systems) technology. The sensor consists of two identical quadratic silicon-nitride/oxide membranes with a length of 1.6 mm. The total thickness of the membrane is 2 μm. The membranes are mounted on a 300 μm thick silicon frame.
- 11. Standard and HighTemperature Sensors 11 UFS UFH Sample area: 0.5 mm2 0.08 mm2 Coating material: aluminum gold Temperature sensor: 8 thermocouples 2 thermocouples
- 12. Metastable Materials ▪ Polymers ▪Polymorphic substances ▪ Metallic alloys ▪ Glass formers ▪ Many composites The structure of such materials depends on the cooling conditions used when they were prepared or produced. On heating, reorganization can occur. This is the reason why the conventional DSC curve does not always correspond to the structure of the original sample. 12
- 13. FDSC Basics: Variationof Heating Rate Examples of reorganization processes: - Separation or elimination of phases - Melting of unstable crystallites with formation of more stable crystals - Transitions of polymorphic phases 13 Reorganization is often determined by kinetic processes and is therefore time dependent. The possible influence of reorganization on the heating curve can be detected by varying the heating rate of the Flash DSC over a wide range. J.E.K. Schawe Thermochim. Acta 603 (2015) 85-93
- 14. FDSC Basics: Variationof Cooling Rate ▪ The formation of structure can be investigated by performing measurements at different cooling rates. ▪ In particular, technical processes carried out at high cooling rates can be simulated using Flash DSC. ▪ Information is obtained about the effect of additives such as nucleating agents under near-process conditions. ▪ The kinetics of transformation can be investigated in a wide time or scanning rate range of several orders in magnitude. Injection molding equipment for polymer processing 14
- 15. FDSC Application Areas Detailedanalysis of structure formation processes in materials. Direct measurement of fast crystallization processes Determination of the stability of glasses Measurement of the reaction kinetics of fast reactions Investigation of the mechanism of action of additives under near-production conditions Comprehensive thermal analysis of materials in a very short time Analysis of very small amounts of sample Determination of physical data for simulation calculations 15
- 16. Application 1 Meltingof PET 16 UserCom 32 p. 12-16 0
- 17. Application 1 Meltingof PET 17 0.1 K/min 10 K/min 200 K/min 3 000 000 K/min
- 18. Application 2 Crystallizationof iPP 18 J.E.K. Schawe, J. Thermal. Anal. Calorim. 116 (2014) 1165-1173 0
- 19. Application 2 Crystallizationof iPP 19 J.E.K. Schawe, J. Thermal. Anal. Calorim. 116 (2014) 1165-1173
- 20. Application 3 Isothermalcrystallization 20 UserCom 32 p. 12-16 0
- 21. Application 3 Isothermalcrystallization 21 Non-nucleated polypropylene shows a bimodal crystallization behavior. The nucleating agent accelerates the crystallization at crystallization temperatures above 30 °C. J.E.K. Schawe, F. Budde, I. Alig, Polymer 153 (2018) 587-596 Crystallization time of iPP with and without nucleating agent
- 22. Application 4 CoolingCurves of BMG 22 The critical cooling rate of the gold based BMG is 500 K/s. J. E.K. Schawe, J. F. Löffler, Nature Commun. 10 (2019) 1337 0
- 23. Application 5 IsothermalCrystallization ▪ The isothermal crystallization behavior of a BMG depends on the previous cooling rate. ▪ After cooling at 500 K/s the sample contains nuclei. The heterogeneous nucleation induces continuous crystallization curves for self-doped glasses (SDGs). ▪ During fast cooling (20,000 K/s) no nuclei are formed. The isothermal crystallization curves show sudden peaks. This is an indication of the stochastic nature of the nucleation in chemically homogeneous glasses (CHGs). 23 J. E.K. Schawe, J. F. Löffler, Nature Commun. 10 (2019) 1337 CHG SDG
- 24. Application 5 TTT-Diagram 24 J.E.K. Schawe, J. F. Löffler, Nature Commun. 10 (2019) 1337 TTT-diagram of SDG and CHG
- 25. Application 6 Meltingat High Temperatures 25 Zr-based alloy for 3D-printing 0
- 26. 26 Application 7 Separationof melting and decomposition UserCom 45 (2017) 15-17 0 0
- 27. Application 8 GlassTransition of a Silica Glass 27 J. E. K. Schawe, K.U. Hess, Thermochim. Acta 677 (2019) 85-90 0
- 28. 28 Summary The Flash DSCis the ideal complement to conventional DSC for the characterization of modern materials and optimization of production processes. Fast and variable measurements save time in the analysis and development of materials. The quality of products can be improved through knowledge of structure formation under actual process cooling conditions. This data can be used to optimize material composition, processing conditions, molds, and tools.
- 29. 29 Summary Features and Benefitsof the Flash DSC ▪ Ultra-high heating rates – suppress reorganization processes ▪ Ultra-high cooling rates – allow the formation of materials with defined structural properties ▪ High sensitivity – permits measurements at low heating rates that overlap with conventional DSC ▪ Wide temperature range – perform measurements from –95 to 1000 °C ▪ Gas-tight measuring head – investigate samples under defined atmospheres ▪ Fast response sensor – enables the kinetics of extremely fast reactions or crystallization processes to be studied ▪ Simplicity of use – From easy sample preparation and sensor change to convenient result evaluation ▪ Oxygen-free environment – protects your sample against oxidation ▪ User-friendly ergonomics – for easy and quick sample preparation and sensor change
- 30. More Information: Related articlesin Thermal Analysis UserCom UserCom articles can be downloaded from www.mt.com/ta-usercoms The revolutionary Flash DSC 1: maximum performance for metastable materials UserCom32 Practical aspects of the Flash DSC 1: Sample preparation for measurements of polymers. UserCom36 Differentiation between two polypropylene samples using Flash DSC UserCom38 Curve interpretation, Part 2: Variation of heating and cooling rates UserCom39 Separation of melting and decomposition using high heating rates UserCom41 Use of the Flash DSC to determine the glass transition temperature of crystalline materials that decompose during melting UserCom45 Strategies for separating overlapping effects, Part 1: DSC UserCom45 Detection of previously unknown menthol polymorphs by Flash DSC UserCom46 Flash DSC measurements of amorphous-crystalline phase transitions of Se1-xTex alloys UserCom 47 Influence of calcium carbonate on the crystallization kinetics of polypropylene at high supercooling UserCom48 Fast Scanning DSC: Selected application examples UserCom49 30
- 31. 31 For More Informationon Thermal Analysis ▪ Webinars: www.mt.com/ta-webinars ▪ E-Training: www.mt.com/ta-etraining ▪ Training: www.mt.com/ta-training ▪ Handbooks: www.mt.com/ta-handbooks ▪ Applications: www.mt.com/ta-applications ▪ TA App: www.mt.com/ta-app ▪ Videos: www.mt.com/ta-videos ▪ Thermal analysis in general: www.mt.com/ta ▪ News: www.mt.com/ta-news
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- 33. Thank you forparticipating! CLICK HERE to learn more and watch the webinar Jürgen Schawe, PhD Senior Scientist, Thermal Analysis Mettler Toledo