Fiber characterization using DSC

1. BAHIR DAR UNIVERSITY
EiTEX
Fiber Chemistry and Physics
Seminar on
Fiber Characterization by using Differential Scanning Calorimetry (DSC)
Submitted to:- Adane H.(ASSoc. Professor)
Febu. 2021 G.C
Prepared By:- Berihun Gashu (MSC in TC)

3. Introduction
Theoretical background of DSC
Basic working principles of DSC
Interpretation of data and analysis of DSC
Characterization on selected fiber
Summary
References
Contents
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4. Thermal analysis (TA) is a group of analytical techniques that used
to analysis the time and temperature at which physical or chemical
changes occur when substance is subjected to cooling or heating.
It is used to measure some properties of textile fibers.
Thermal Analysis?
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5. Common Thermal Analysis Techniques
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Differential Mechanical Analysis (DMA), Modulus
Thermo Gravimetric Analysis (TGA), Mass
Differential Scanning Calorimetery (DSC), Heat flow
Thermo Mechanical Analysis (TMA), Dimension
Differential thermal analysis (DTA), Mass and Heat flow

6. Theoretical background of DSC
The difference in heat flow to the Specimen and Reference at
the same temperature is recorded as a function of temperature.
Provides heat flow in to sample and out of sample.
Temperature range from -120 to 725◦C.
Differential scanning calorimetry(DSC)
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Endothermic heat flow? Tg, Tm, Evaporation
Exothermic heat flow ? Tc, oxidation, cure

7. What Type of technologies DSC use?
1. Heat flux DSC
The test sample and reference material are enclosed in the single
furnace together.
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Sensor
heater

8. 2. Power compensation DSC
The specimen and reference temperatures are controlled independently
using separate ovens.
The energy difference is plotted as a function of sample temperature.
7
Sensor
heater

9. What is basic working Principles of DSC?
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10. 9

11. 1. switch on
o nitrogen valve, DSC, cooling and desktop
2. Stabilize the apparatuses for 30 min
3. Sample preparation
oPut the sample and reference on heater
4. Start the run
5. Analyze the Data
Operational Procedure
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12. Pans, aluminum alloy, platinum, stainless steel and
silver.
It can be open, pin-hole, covered or sealed
Its size of the sample should be 0.5mg to 100mg.
Small sample pans (0.1 mL).
Material should completely cover the bottom of
the pan .
Avoid overfilling (minimize thermal lag).
How can a Sample Prepared?
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13. 1. Temperature
2. Weight balance
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How to Calibrate DSC?

14. What can DSC measure? :-
a. Glass transition temperature (Tg)
b. Crystallization temperature (Tc)
c. Melting temperature (Tm)
d. Polymers crystallinity determination
Interpretation of DSC data and analysis
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15. a. The Glass Transition Temperature
Tg: amorphous material undergoes a transition from a brittle or hard state
to a rubber-like viscous state.
Peaks will show an sudden and linear decrease
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Endothermic

16. Polymers will give off enough energy to move into very ordered arrangements, which is
called crystals. (exothermic)
Here there is latent heat of crystallization
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b. Crystallization Temperature
Exothermic peak
Cooling after rubbery state

17. similar in size to the corresponding melting point
peaks.
Some differences may appear as a result of super
cooling but the peak area should not deviate by
more than 20%.
Crystallization Point Peak Examples
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Heat
flow
endo
up(mW/m2)

18. As a solid sample melts to a liquid, it will require more heat flowing to
the sample to increase its temperature at the same rate as the reference.
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c. Melting Temperature
Endothermic peak
heat flowing after crystalline

19. 18
Peak broadness/Sharpness
Tm
Purity

20. DSCCurve
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Putting it all together

21. d. Polymers Crystallinity Determination
Properties of polymers like comfort, strength and
absorbency are highly affected by percent
crystallinity.
Polymer Hm° (J/g)
Nylon 6 230.1
Nylon 6,6 255.8
PET 140.1
Polypropylene 207.1
Polyethylene 293.6
Polylactic acid 93.1
Reference value (The heat of melting if the
polymer were 100% crystalline).
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22. Characterization of Nylon 6 by DSC
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Characterization on selected fiber
Endo
up

23. Nylon 6 Crystallinity Determination
 From the DSC of
Nylon 6 We have
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24. Characterization of PET by DSC
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Endo
up

25. Characterization of Poly Lactic Acid by DSC
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26. Poly Lactic Acid Crystallinity Determination
 From the DSC of Poly
Lactic Acid We have
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27. DSC measures the energy required to keep both the reference and the
sample at the same temperature.
DSC an important tool in the experimental characterization of
polymeric materials.
DSC measures the heat capacity of a sample by recording the heat
flow rate into the sample and comparing it to a reference sample.
From the DSC curve one can determine materials transition points
like Tg, Tc and Tm.
It determine the degree of crystallinity for thermoplastic materials.
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Summary

28.  DEMIREL, B., YARAS, A., & ELCICEK, H. (2011). Crystallization Behavior of PET Materials . BAU Fen Bil. Enst.
Dergisi Cilt , 26-35.
 Gurudeep R.Chatwal, Sham K.Anand, Instrumental Methods of Chemical Analysis, Thermal Methods, 5 th edition. (pg
no:2.747- 2.753)
 Mutlur, S. Thermal Analysis of Composites Using DSC. In Advanced Topics in Characterization of Composites (pp. 11-33).
 Perkin Elmer. (2013). Differential Scanning Calorimetry (DSC). Waltham: Perkin Elmer.
 B.K.Sharma, Instrumental Methods of Chemical Analysis, Thermoanalytical methods, 26th edition, goel publishing house,
Meerut,2007. (pg.no.308)
 Sichina, W. (2000). DSC as Problem Solving Tool: Measurement of Percent Crystallinity of Thermoplastics. Norwalk: Perkin
Elmer.
 Demonstration of MEMS-based differential scanning calorimetry for determining thermodynamic properties of biomolecules.
Sensor Actuat B-Chem 2008;134:953– 958
References
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29. Thank You for
your
kind attention!
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