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PRESENTED BY MALLIKA JOLLY

UNDER THE GUIDANCE OF
Dr.(Mrs).VARSHA POKHARKAR
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ñ A branch of materials science where the
properties of materials are studied as they change with
temperature.
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ë DTA ʹ temp. diff.
ë DSC - enthalpy
ë TGA ʹ mass
ë TMA - deformation
ë DMA ʹ deformation
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0Gide temperature range
0Any physical form of sample can be accommodated using variety of vessels
0Small amount of sample is required (0.1ʅg-10mg)
0Atmosphere in vicinity of sample can be standardized
0Time required can range from several minutes to several hours
0Instruments are priced resonably

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u DTA measures temperature difference between a sample
and an inert reference (ºm
mm ) while heat flow to the
reference and the sample remains the same
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uFurnace temperature is recorded as a function of time

uMinimum ȴT measured by DTA : 0.01K

uCrystallization: exothermic
uMelting: endothermic
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uThe sample and reference are maintained at the same temperature,
even during a thermal event (in the sample)
uDSC measures the energy required to maintain zero temperature
differential between the sample and the reference(ȴd½

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DSC- calorimetric method, energy differences measured.
DTA- temperature differences measured.
The applications of both techniques are similar, but DSC is now more
popular.
DTA is used for higher temperature and qualitative applications.
DSC is used for calorimetric determinations, sample purity
determinations and kinetics
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Difference in heat flow into S and R is measured with (linear) change in sample
temperature.
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S and R heated by separate heaters to keep same temperature, as T is changed
linearly
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uaccurately-weighed samples (~3-20 mg, usually 3-5 mg for simple
powders) small
usample pans (0.1 mL) of inert or treated metals (Al, Pt, stainless)
u several pan configurations, e.g., open , pinhole, or hermetically-sealed
pans
usame material and configuration should be used for the sample and the
reference material should completely cover the bottom of the pan to
ensure good thermal contact
uavoid overfilling the pan to minimize thermal lag from the bulk of the
material to the sensor
u small sample masses and low heating rates increase resolution, but at
the expense of sensitivity
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Packing schemes for open type
and hermetically sealed-type
sample vessels. Only samples I
and IV are correctly packed
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Endothermic events Exothermic events Baseline shifts
melting Crystallization glass transition
Sublimation Decomposition
Desolvation chemical reactions
chemical reactions solid-solid transitions
solid-solid transitions

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uSample may react with air - oxidising or burning
uControl moisture content of atmosphere
uUse inert gas e.g. nitrogen or argon
uFlowing purge gas
uIn some cases deliberately choose reactive gas, e.g.
ʹ hydrogen to reduce an oxide to metal
ʹ carbon dioxide which affects decomposition of metal carbonate
uRemoves waste products from sublimation or decomposition
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uExamines the mass change of a sample as a function of
temperature in the scanning mode or as a function of time in the
isothermal mode.

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uTG curves are recorded using a thermo balance
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ü sample identification;
ü form and dimensions of sample;
ü mass of sample, initial and final;
ü preconditioning of sample;
ü crucible shape, size and material;
ü type and position of sample thermocouple;
ü atmosphere and gas flow rate;
ü heating rate or isothermal temperature;
ü reference material used for temperature calibration;
ü type of instrument used.
  
 


 
uGlass Transition Temperature
uMelting Point
uHeat Capacity Measurement by DSC
uPurity Determination by DSC
uCrystallinity Determination by DSC
uPolymorphism
uPhase Transition
uGel- Sol Transition
uTemperature measurement
uEnthalpy measurement
uReaction rate kinetics
uMolecular Rearrangement during Scanning
uAnnealing
uBound Gater Content
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Physical properties that undergo changes at Tg:
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Baseline change h occurs for substances with different Cp, or for same
substance after phase change.
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Peak width a valuable

measure of purity:

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Polymers

Crystalline Amorphous
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uPolymorphism is the term used to describe the occurrence of different
structural forms of a material,
and is observed in polymers such as polyamides, polypropylene,
polysaccharides and fluorinated polymers.
uX-ray diffractometry is the principal technique used to probe the
polymorphic nature of polymers.
uThe temperature and enthalpy change associated with crystal to crystal
transitions are measured using DSC.

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A phase diagram is a graphical representation of the relationship
between a given set of experimental parameters and the phase changes
occurring in a material. Sample volume, transition temperature and
enthalpy, pressure and composition of the material are commonly used
parameters in phase diagrams
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Polymer chains can form infinite networks by either physical or chemical
association. Reversible networks in the presence of a solvent form
reversible gels. The cross-links between individual chains in a reversible gel
are localized, but not permanent, and the interacting groups dissociate and
reassociate according to the conditions of thermodynamic equilibrium. The
gel structure present at low temperatures is transformed on heating and a
liquid state is observed. This process, which can be reversed on cooling, is
called the gel-sol transition.
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Heat Flux DSC ñ
  

Dialatometer ñ m  
 
  
Laser Flash apparatus ñ m 
 
Dynamic Mechanical Analyzer ñ 





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Expansivity è 

 

  
  
uApparent specific heat (specific heat and overlapped transition
enthalpies) of the PTFE
uThermal diffusivity of the PTFE
uThermal conductivity of PTFE=
 
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