THERMAL

ANALYSIS

Presented By:
Saadia Ashraf Qureshi 04
Sidra Shaukat 11
Samia Yousaf 22
Sanam Bahadur 40
Zunaira Tufail 18
Definition
Thermal Analysis is a branch of materials science by which the
physical, chemical , and mechanical properties of materials are
studied as a function of temperature. This measurement provides
information about physical phenomena, such as phase transitions,
absorption, adsorption and desorption; as well as chemical
phenomena including thermal decomposition, and solid-gas
reaction
Methods of Thermal Analysis

Thermo Gravimetric
Analysis (TGA)

Thermal Stimulated Dynamic Mechanical Analysis

Current (TSC) (DMA)

Dynamic Mechanical
Thermal Analysis
(DMTA)
 Thermo Gravimetric Analysis (TGA)

Principle
 Upon heating a certain material, its weight increases or decreases due to certain
reactions like decomposition, oxidation and dehydration.
 It measures the change in mass or weight in function with the temperature or
time with constant heating rate or constant time.
 TGA is based on that the sample is continuously weighted as temperature is
elevated using an instrument called “thermo balance”.
 Data is recorded in the form of curve called “thermo gram”.
 Instruments which can quantify loss of water, loss of solvent, loss of plasticizer
are used and comparing weight loss of material is being followed
 Thermo Gravimetric Analysis (TGA)

Types
 Dynamic (scanning mode) TGA
This type of analysis the sample is subjected to conditions of continuous
increase in temperature usually linear with time.

 Static (Isothermal ) TGA:

This type of analysis the sample is maintained at a constant temperature for a
period of time during which any change in we
 Thermo Gravimetric Analysis (TGA)

Instrument Thermo Balance

Components of thermo balance:
 The balance (electronic micro balance)
 The furnace (heart)
 The programmer (brain)
 The recorder (data collector)
Thermo Gravimetric Analysis (TGA)
 Thermo Gravimetric Analysis (TGA)

Factors Affecting TGA Curve

Instrumental factors:
 Furnace heating rate
 Furnace atmosphere 

Sample characteristics:
 Weight of sample
 Sample particle size
 Thermo Gravimetric Analysis (TGA)

Applications

 Materials characterization through analysis of

characteristic decomposition patterns.

 Can be used to evaluate the thermal stability of a material

in a desired temperature range.

 Can determine the inorganic or organic content in the

sample
 Thermo Gravimetric Analysis (TGA)

Useful Information
 Decomposition temperatures
 Quantitative weight losses
 Compositional analysis
 Long term stabilities
 Flammability properties
 Rates of degradation
 Life time of a product
 Effect of reactive or corrosive atmospheres
 Oxidative stability of material
 Dynamic Mechanical Analysis (DMA)

Principle
 A sinusoidal strain (oscillating force) is applied to the material at a given
frequency, while the temperature is ramped up or down over a range and
deformation is recorded.
 −50°C and 220°C for polymers
 25°C and 600°C for glasses and ceramics
 50°C and 600°C for metals
 Sinusoidal motion is the repeated motion in which the dynamic clamp
repeated the same movement over and over with maximum and minimum
values of forces
 Dynamic Mechanical Analysis (DMA)

Instrument DM Analyzer
 Dynamic Mechanical Analysis (DMA)

Useful Information
Through DMA, some useful properties
of materials can be measured, such as
 Viscoelasticity
 Dynamic Elastic Modulus (E’)
 Glass Transition Temperature (Tg)
 Damping Behavior
 Creep Recovery Behavior .
Dynamic Mechanical Analysis (DMA)
 Dynamic Mechanical Analysis (DMA)

Glass Transition Temperature (Tg)

 The temperature at which the
maximum in the tan delta peak is
observed.

 It defines the point at which the

material transitions from an
elastic to a rubbery state
 Thermally Stimulated Current (TSC)

Principle
 TSC studies are usually conducted to provide additional information about
molecular mobility in the solid state, and as a result characterize phase
transitions that are related to thermal transitions in the crystalline
(polymorphic) and amorphous phases

 TSC is a thermoelectrical analytical method , in which the sample is subject

to constant electrical field and the current through a sample is measured as a
function of temperature

 AN electric field is applied to a sample while it is heated to a temperature in

which the molecule mobility is high followed by cooling
 Thermally Stimulated Current (TSC)

Instrument Spectrometer
A different model, Holmarc’s TSC spectrometer is
used to study energy levels in semiconductors or 
insulators, especially solar cells. The sample energy
levels are first filled by exposing it to a halogen lamp
light source for a user specified time. The
temperature of the sample at this time can be set as
low as 70°C. The sample can then be heated
gradually up to 150°C at a specified ramping rate,
which causes emission of electrons and holes in the
sample.
 Thermally Stimulated Current (TSC)

Example
Caffeine exists in two enantiotropic polymorphic forms (form I and form II)
implying that there is a clear transition point (temperature) at which one
polymorph converts into the other. The TSC data indicate clear differences
between the two forms.
 Thermally Stimulated Current (TSC)

Application
 TSC is a new tool that also can be used to analyze pharmaceutically important molecules.
 TSC studies are usually conducted to provide additional information about molecular mobility
in the solid state.
 Main use of TSC is to study relaxation processes such as glass transition.
 TSC has been used to distinguish between two different polymorphic forms and amorphous
phase.
 TSC is applicable to study various materials, such as :
 Semiconductors
 Semimetals
 Polymers
 Plastics
 Biaxial films
 Polymer-clay composites
 Amorphous materials.
Dynamic Mechanical Thermal Analysis (DMTA)

Defination
 Characterize Visco-Elastic properties.

 Storage Modulus E’ (elastic response) and Loss Modulus E’’ (viscous response) of polymers are
measured as a function of T or time as the polymer is deformed under an oscillatory load
(stress) at a controlled (programmed) T in specified atmosphere.

 DMTA can be applied to determine the glass transition of polymers or the response of a
material to application and removal of a loa
Dynamic Mechanical Thermal Analysis (DMTA)

Instrument
Dynamic Mechanical Thermal Analysis (DMTA)

Principle
 DMA is based on two important concepts of stress and strain.
 Stress σ = F/A
 Stain γ = ∆Y/Y
 The modulus (E), a measure of stiffness, can be calculated from the slope of the stress-
strain plot. This modulus is dependent on temperature and applied stress.
 DMA instruments apply sinusoidally oscillating stress to samples and causes sinusoidal
deformation. The relationship between the oscillating stress and strain becomes
important in determining viscoelastic properties of the material.
 Stress and strain can be expressed with:
 Where, σo = maximum stress applied
 ω = frequency of applied stress, and t =time
 Dynamic Mechanical Thermal Analysis (DMTA)

 The applied stress and measured strain

are in phase for an ideal elastic material.
 The stress and strain are 90o out of phase
for a purely viscous material.
 Viscoelastic materials have a phase lag less than 90o .
 The phase angle between the stress and strain tells us a great deal about the viscoelasticity
of the material.
 For one, a small phase angle indicates that the material is highly elastic; a large phase
angle indicates the material is highly viscous.
 The elastic response of the material is analogous to storage of energy in a spring, while the
viscosity of material can be thought of as the source of energy los
Dynamic Mechanical Thermal Analysis (DMTA)
Working
The sample is clamped into a frame and is heated by
the furnace. The sample in the furnace is applied the
stress from the force generator via probe. To make the
strain amplitude constant, the stress is applied as the
sinusoidal force. The deformation amount generated
by the sinusoidal force is detected. Viscoelastic values
such as elasticity and viscosity is calculated from the
applied stress and the strain and plotted as a function
of temperature or time.
 Dynamic Mechanical Thermal Analysis (DMTA)
Types of Dynamic Experiments
Temperature Sweep Frequency Scans
 The frequency and amplitude of  It tests a range of frequencies at a constant temperature to
oscillating stress is held constant while analyze the effect of change in frequency on temperature
the temperature is increased. riven changes in material.
 The results of temperature sweeps  This type of experiment is typically run on fluids or polymer
are displayed as storage and loss melts.
moduli as well as tan delta as a
 The results are displayed as modulus and viscosity as
function of temperature
functions of log frequency.

Time Scans
 The temperature of the sample is held constant, and properties are measured as functions of time.
 This experiment is commonly used when studying curing of thermosets, materials that change chemically upon
heating.
 Data is presented graphically using modulus as a function of time; curing profiles can be derived from this
information.
Dynamic Mechanical Thermal Analysis (DMTA)
Dynamic Mechanical Thermal Analysis (DMTA)

 Advantages:
 Dynamic mechanical analysis is an essential analytical technique for determining the
viscoelastic properties of polymers.
 Due to its use of oscillating stress, this method is able to quickly scan and calculate the
modulus for a range of temperatures.
 This analytical method is able to accurately predict the performance of materials in
use.
 Fast analysis time (typically 30 minutes).
 Easy sample preparation.
Dynamic Mechanical Thermal Analysis (DMTA)
 Applications:
 Characterization of printed circuit board materials by DMA.
 It finds application in Research and Development for material lifetime predictions.

 Limitations:
 The modulus value is very dependent on sample dimensions, which means large
inaccuracies are introduced if dimensional measurements of samples are slightly
inaccurate.
 Oscillating stress converts mechanical energy to heat and changes the temperature of
the sample.