Thermal Analysis

2
Nomenclature of Thermal Analysis
- Thermal analysis is a group of techniques
that study the properties of materials as
they change with temperature
- Gives properties like Enthalpy, Thermal
capacity, Mass change, Co-efficient of
thermal expansion.
- For studying reactions in solid state,
thermal degradation reactions, phase
transitions.
3
Techniques
Thermal Gravimetric Analysis (TGA): mass
Weight Loss due to decomposition
Differential Thermogravimetric Analysis (DTG)
Differential Scanning Calorimetric (DSC): H
Heat flow during Transitions
Thermal Mechanical Analysis (TMA): deformation/dimension
Thermal Expansion Coefficient
Temperature Programmed Desorption (TPD): evolved gas
Temperature at which gas is desorbed from (catalyst) surface
4
Principle
Sample is heated at a constant heating
rate
Samples property is measured
Weight TGA
Size TMA
Heat Flow DSC
Gas evolved TPD
5
Thermo Gravimetric Analysis (TGA)
Constant Heating Rate
Heating Rate (C/min)
Data
Weight vs Time
Weight vs Temp
TGA curve gives information
on:
Change in sample composition
Thermal stability
Sample amount: 5-20 mg
Heating rate: 1-100 C/min
http://www.netzsch.com/
6
TGA: Decomposition of CaC
2
O
4
.H
2
O
- H
2
O
- CO
- CO
2
Air, 10 K/min
7
http://www.netzsch.com/
8
TGA: Phenomena causing m
9
TGA: Applications
Characterizing Thermal stability, Material
purity, humidity determination
Examination of Corrosion studies
10
TGA/MS (Mass Spectrometry)
MS characterizes substances by identifying and
measuring intensity of fragment ions of different
mass-to-charge ratio (m/z)
Incoming gas molecules are first ionized and
then separated according to their m/z
11
http://www.netzsch.com/
12
Factors affecting TG curve
13
Differential Scanning Calorimetry (DSC)
A Calorimeter measures heat into or out of a sample
A Differential Calorimeter measures the heat of a
sample relative to a reference
A Differential Scanning Calorimeter does the above
with a temperature or time scans
Operates by comparing the heat transfer to the sample
pan with the heat transfer to a reference pan
Separate heaters heat pans at same rate
Sample pan with material will take more heat to keep T
of sample pan increasing at the same rate as reference
pan
14
DSC, Heat Capacity
15
DSC: Principle of Operation
T
f
Time
or T
r
Heat flow (mW)
0
-10
DSC signal,
Peak integral -> H
H
Temperature
T
r
T
s
T
f
Time
16
DSC cell
Sample pan (Al / Cu / Au)
17
Sample Preparation: Shape
Keep sample as thin as possible (to minimize
thermal gradient)
Cover as much of the pan bottom as possible
Sample should be cut rather than crush
18
DSC Thermogram: Typical Transitions
Exo
Endo
Glass
transition
Crystallization
Melting
Endo
a polymer
19
To characterize polymers, organic
chemicals, inorganics
Tg, melting, crystallization, onset of
oxidation and heat capacity
DSC: Applications