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Thermal Analysis

SSK 4242
The Effect of Heat on Materials
Very important to human life – why ??? i) Weaker intra-molecular force

The effect of heat on materials: change in


molecular and atomic vibration and ionic movement



Structural or shape change
Melting

• Decomposition a) CaCO3(s) CaO(s) + CO2(g)
• Sintering b) NH4Cl(s) NH3(g) + HCl(g)
• evaporation

Oxidation: ii) Weaker inter-molecular force


2Ag(s) + ½O2 Ag2O(s)
4Al(s) + 3O2 2Al2O3(s)
C(s) + O2(g) CO2(g)
PbS(s) + 3O2(g) 2PbO(s) + 2SO2(g)

a) BaCl2.2H2O(s) BaCl2(s) + 2H2O(g)
Reduction:
b) CuSO4.5H2O(s) CuSO4(s) + 5H2O(g)
a) CuO(s) + H2(g) Cu(s) + H2O(g)
b) SnO(s) + H2(g) Sn(s) + H2O(g)
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Thermal Analysis
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Thermal Events
In case more than one solid materials involved
in the heat treatment, more thermal events will
take place leading to:

• the formation of solid solution;


• the formation of an eutectic mixture;
• the formation of a new compound.
Table 1.1 Summary of the
heat effect on materials
Formation of a new compound:

Fe2O3(s) + MgO(s)
MgFe2O4(s) Table 1.2 The effect of
heat on solid materials

Double Decomposition:

NaCl(s) + AgBr(s)
AgCl(s) + NaBr(s)

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Heat Capacity

All materials have their own heat capacities

…an ability for the materials to absorb and keep the heat energy …

Mechanisms of retaining heat energy:

a) Solid materials The heat energy is kept via atomic vibration about
a min position around the atom in the lattice

b) Metallic materials The heat energy is also kept via the electronic
movement of the metal

c) Liquid materials The heat energy is kept via the rotational


movement of the atoms, therefore liquids
generally have greater heat capacity than the
solid materials.

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Heat Capacity (Cp)
…the amount of heat that is required to raise the temperature of a body by 1 Kelvin…

• The absorbed heat is stored as enthalpy


• Cp is also a measure of the amount of enthalpy change when the body
temperature is raised by 1 Kelvin

Cp = H / T

Table 1.3 Parameters and


techniques in the
measurement of heat effect

Definition of Thermal Analysis:


Thermal analysis is defined as a group of techniques
where the properties of samples are monitored versus
time or temperature while the sample’s temperature is
controlled under certain atmosphere
International Confederation for Thermal Analysis and Calorimetry (ICTAC)

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Thermal Analysis
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Temperature Control Programme


a) Heating or cooling at a constantly changing temperature
b) Heating at a constant temperature
c) Combination of (a) and (b) above.

Sample
• The material that is placed in the instrument at the beginning of
the experiment
• The reaction products

Thermogram
• The thermal analysis curve
• The experimental data in a graphic form

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Differential Thermal techniques:


These Involve measurement of the differential properties/values
between samples and the reference materials
Example: the differential thermal analysis (DTA) where the measured
parameter is the difference between the sample temperature
and the reference temperature

Derivative Thermal techniques:


These involve measurement or calculation of mathematical
derivation versus time

Example: the derivative thermogravimetry (DTG) that involves


measurement of the rate of mass loss (dm/dt) plotted versus
temperature, T.

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Measurement of Heat Effect


• Sample
• Reagent (Heat)
• Signal

Signal
Sample generating Heat
unit

Signal

Information about the sample

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Thermal Analysis
Thermal Analysis Techniques, the Measured SSK 4242
Parameters and the Thermograms
The rate of mass change versus
the temperature change
Mass loss m / T
m

T T

a) Thermogravimetry (TG) b) Derivative Thermogravimetry (DTG)

The temperature difference between the


sample and the reference versus the
temperature change Heat flow versus the
temperature change
T
H / T

T
T
c) Differential Thermal analysis (DTA) d) Differential Scanning Calorimetry (DSC)
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Thermal Analysis
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Conditions for Heat Effect Measurement

1. Measurement of the physical properties and the


sample temperature should be made
continuously,
2. Measurement and recording of both parameters
should be made automatically,
3. The temperature change of the sample
(increased or reduced) takes place at a constant
rate.

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Application of Thermal Analysis


Some examples of materials that can be studied by Thermal Analysis Methods

Asbestos Glass Catalysts


Liquid crystal Ceramics Metals and steels
Clay Minerals Explosives
Organic materials Inorganic chemicals Fats, oils and waxes
Organometallics Fertilizers Pharmaceuticals
Fuels Plastics Rubber
Textiles Foods Plant materials

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