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