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Thermal Analysis of Polymers By Muhammad Zafar Iqbal P.E. Physical Properties of Polymers
Agenda ,[object Object],[object Object],[object Object],[object Object],[object Object],06/10/09 Polymer & Process Engineering
Thermal Analysis ,[object Object],[object Object],[object Object],[object Object],[object Object],[object Object],[object Object],[object Object],[object Object],06/10/09 Polymer & Process Engineering
Characteristics of TA techniques ,[object Object],[object Object],[object Object],[object Object],[object Object],[object Object],[object Object],[object Object],06/10/09 Polymer & Process Engineering
[object Object],[object Object],[object Object],06/10/09 Polymer & Process Engineering
06/10/09 Polymer & Process Engineering
Variants of DSC ,[object Object],[object Object],[object Object],[object Object],[object Object],[object Object],[object Object],[object Object],[object Object],[object Object],[object Object]
DSC 06/10/09 Polymer & Process Engineering
Heat Flux DSC Set-up is similar to DTA: analysis sample and reference sample. Heat-Flow DSC : each sample is surrounded by an inner ring and an outer ring of thermocouples.  The average temperature difference between the two measures the heat flow into or out of the sample. Outer ring of 30 thermocouples Inner ring of 30 thermocouples Reference Analysis
Output of DSC Temperature, K Thermogram dH/dt, mJ/s Glass transition crystallization melting exo endo
Glass Transition ,[object Object],[object Object],[object Object],[object Object],Temperature, K Thermogram dH/dt, mJ/s Glass transition T g
Crystallization ,[object Object],[object Object],[object Object],[object Object],[object Object],Temperature, K Thermogram dH/dt, mJ/s Crystallization T c
Melting ,[object Object],[object Object],[object Object],[object Object],Temperature, K Thermogram dH/dt, mJ/s Melting T m
Conclusion
Sampling ,[object Object],[object Object],[object Object],[object Object],[object Object],[object Object],[object Object],[object Object]
Crucibles Choice of crucible is critical. •  Thermal properties of crucible.  •  Reactive properties with samples. •  Catalytic behaviour with samples. Aluminum:  inexpensive, low temp Copper : used as catalyst (testing polymers) Gold : higher temp, expensive Platinum:  still higher temp, expensive. Alumina  (Al 2 O 3 ): very high temp Sapphire : crystalline alumina, more chemically resistant than amorphous Al 2 O 3 .
Calibration ,[object Object],[object Object],[object Object],[object Object],[object Object],[object Object],[object Object],[object Object],[object Object],[object Object],[object Object],[object Object],[object Object],[object Object],[object Object],[object Object],[object Object],[object Object],[object Object],[object Object],[object Object],[object Object],[object Object],[object Object],[object Object]
What Can You Measure with DSC? ,[object Object],[object Object],[object Object],[object Object],[object Object],[object Object],[object Object],[object Object]
Most Important to Remember 06/10/09 Polymer & Process Engineering
Where Used? ,[object Object],[object Object],[object Object],[object Object],[object Object],[object Object]
Poly (Lactic Acid) Glass transition temperature, T g .
DSC traces for melting and crystallization of a polymer sample .
DSC traces of Low Crystallinity PLA treated in Water at 70  C and 100  C. The higher the crystallinity achieved at 100   C, the higher and the less defined the T g
Melting of two semicrystalline HDPE samples.
[object Object],[object Object],[object Object]
Sample Preparation 06/10/09 Polymer & Process Engineering
06/10/09 Polymer & Process Engineering
Temperature Gradient in Sample 06/10/09 Polymer & Process Engineering
Mass of Sample 06/10/09 Polymer & Process Engineering
Why should we work on micro level..? 06/10/09 Polymer & Process Engineering
Sample Packing 06/10/09 Polymer & Process Engineering
06/10/09 Polymer & Process Engineering
Scanning Rate 06/10/09 Polymer & Process Engineering

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Ppp Dsc 1 Thermal Analysis Fundamentals Of Analysis

  • 1. Thermal Analysis of Polymers By Muhammad Zafar Iqbal P.E. Physical Properties of Polymers
  • 2.
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  • 6. 06/10/09 Polymer & Process Engineering
  • 7.
  • 8. DSC 06/10/09 Polymer & Process Engineering
  • 9. Heat Flux DSC Set-up is similar to DTA: analysis sample and reference sample. Heat-Flow DSC : each sample is surrounded by an inner ring and an outer ring of thermocouples. The average temperature difference between the two measures the heat flow into or out of the sample. Outer ring of 30 thermocouples Inner ring of 30 thermocouples Reference Analysis
  • 10. Output of DSC Temperature, K Thermogram dH/dt, mJ/s Glass transition crystallization melting exo endo
  • 11.
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  • 16. Crucibles Choice of crucible is critical. • Thermal properties of crucible. • Reactive properties with samples. • Catalytic behaviour with samples. Aluminum: inexpensive, low temp Copper : used as catalyst (testing polymers) Gold : higher temp, expensive Platinum: still higher temp, expensive. Alumina (Al 2 O 3 ): very high temp Sapphire : crystalline alumina, more chemically resistant than amorphous Al 2 O 3 .
  • 17.
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  • 19. Most Important to Remember 06/10/09 Polymer & Process Engineering
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  • 21. Poly (Lactic Acid) Glass transition temperature, T g .
  • 22. DSC traces for melting and crystallization of a polymer sample .
  • 23. DSC traces of Low Crystallinity PLA treated in Water at 70  C and 100  C. The higher the crystallinity achieved at 100  C, the higher and the less defined the T g
  • 24. Melting of two semicrystalline HDPE samples.
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  • 26. Sample Preparation 06/10/09 Polymer & Process Engineering
  • 27. 06/10/09 Polymer & Process Engineering
  • 28. Temperature Gradient in Sample 06/10/09 Polymer & Process Engineering
  • 29. Mass of Sample 06/10/09 Polymer & Process Engineering
  • 30. Why should we work on micro level..? 06/10/09 Polymer & Process Engineering
  • 31. Sample Packing 06/10/09 Polymer & Process Engineering
  • 32. 06/10/09 Polymer & Process Engineering
  • 33. Scanning Rate 06/10/09 Polymer & Process Engineering

Editor's Notes

  1. Polymer Reaction Engineering Polymer Reaction Engineering