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7/27/2019 Thermal Analysis of Materials
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Hamzah Mukhtar
Pablo Ramos
Vamakshi Khati
Daniel Gomez
Thermal Analysis of Materials
Group-6
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Contents
PROBLEM
INTRODUCTION TO PRODUCT
DSC
DILATOMETRYDMTA
CONCLUSION
SUMMARY
REFERNCES
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Problem
One Asian customer has a problem with a polymergland that fails after a few months. It is observed that
this polymer has multiple fractures and its surface is a
bit harder than the reference sample. This polymer
cable gland is used in power cable.
There are several factors that are to be considered for
failure of a material.
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Introduction to Product
Polymer cable glands attaches and holds the end of acable to the equipment.
Polymer properties specifically depends on some
specific parameters like Tg, Tm, temperature of
crystallisation, degree of crystallinity and degradation.
So to estimate why the polymer becomes harder and
fractures we have to analyse the characteristics of
polymers using DSC, DMTA and Dilatometry.
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Differential Scanning Calorimetry (DSC)
DSC stands for differential scanning calorimetry is athermo-analytical technique.
It measures the amount of heat absorbed or released
when a sample is cooled or heated and thus providing
the data that is related with them.
DSC chambers consist of two more or less equal
chambers one chamber contains the inert reference
sample (usually alumina) where the heat capacitance is
well defined in more or less all temperature ranges and
in the other chamber is our sample.
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Schematic diagram of a typical differential scanning calorimeter.
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DSC determines the thermal transitions in polymers, by
which we can understand the behaviour of our polymer cable
gland and to compare it with our reference sample. The
information thus collected can determine the changes in the
polymer.
The following diagram shows some changes in our material
and they are showed in endothermic/exothermic reactions.
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Dilatometry It is the thermo-analytical method which is used for the
measurement of shrinkage and expansion of the materialsunder controlled temperature range.
The amount of shrinkage or expansion is dependent on
material properties or characteristics.
By using dilatometry following properties can be measured Thermal expansion and coefficient of thermal expansion
Volumetric expansion
Influence of additives/raw materials
Density change
Glass transition temperature (Tg)
Dilatometric softening point (Td)
Phase transition
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Pushrod dilatometry is a method that is used for determination
of dimensional changes versus temperature or time while
sample is subjected to a controlled temperature program.
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L0=Initial sample
length
T=Change intemperature
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Dynamic Mechanical Thermal Analysis
DMTA or DMA measures the temperature dependent visco-elastic properties along with modulus of elasticity.
Strain is measured by applying fluctuating stress and thus
complex modulus is determined. This approach can be used
to locate the Tg of the material, as well as to identifytransitions corresponding to other molecular motions.
Temperature-sweeping DMA is often used to characterize
the glass transition te
DMA measures the visco-elastic properties by transient ordynamic oscillatory tests temperature of a material.
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Transient tests include stress relaxation and creep. In
dynamic oscillatory test, a sinusoidal stress is applied
and sinusoidal strain is measured along with phase
difference. For polymers the phase difference is
intermediate as in next figure.
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In Asia region these glands used for power cables are made ofpolymers with high content in halogens (for instance PVCcan reach 57% of chloride), this is also a problem because itcould lead to degradation of the polymer easily. Degradationcan occur as a result of the formation and then breakage ofdouble bonds (for instance when a Carbon is bond with ahalogen and it breaks). This occurs in PVC in the presence ofan acid species. Active Hydrogen atoms will remove aChlorine atom from the polymer molecule, formingHydrochloric acid (HCl) causing de-chlorination of adjacent
Carbon atoms. These de-chlorinated Carbon atoms tend toform double bonds which can be broken in an ozoneatmosphere (normal conditions).
Polymer Description
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Conclusion Some mechanisms of hardening are related with
recrystallization, as they will increase the percentage
of crystallinity of the polymer. As a result it will get
harder, and get brittle, which along with stresses could
lead to failure.
Introducing oxygen and carbon atoms in the main
chain will lead to hardening, besides C-C bonds,
oxygen atoms are introduced generating a dipole. The
link will be reinforced so there will be an increase in
resistance to being deformed, so atmospheric
conditions should also be taken into account.
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Conclusions are related then to avoid recrystallization
(be aware of Tg and temperature of recrystallization of
the polymer), take into account atmosphere conditionsand content of halogens in the polymer used.
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Summary
Introduction to polymer glands
Discussed about the Problem to the
product
Methods being used to Analyse the
Problem
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References http://en.wikipedia.org/wiki/Differential_scanning_c
alorimetry
http://en.wikipedia.org/wiki/Differential_thermal_an
alysis
http://www.pslc.ws/macrog/dsc.htm
http://www.mate.tue.nl/mate/pdfs/10367.pdf
http://en.wikipedia.org/wiki/Dynamic_mechanical_a
nalysis
http://en.wikipedia.org/wiki/Polyvinyl_chloride
http://www.files.chem.vt.edu/chem-
dept/marand/Lecture23.pdf