DMA

II
Natural Sciences Tripos Parts II
MATERIALS SCIENCE
C11: Thermal Analysis
Name............................. College..........................
Dr N. A. Rutter
Michaelmas Term 2015-16
2015 16
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Course C11: Thermal Analysis
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COURSE C11
THERMAL ANALYSIS
Thermal Analysis (TA) describes a set of techniques which are widely used in both academic
research and industry. These techniques are generally straightforward to use and are able to
characterise a wide range of materials and materials properties.
This course is an introduction to a number of these techniques, describing how they are performed
and how to interpret the data they produce. In addition practical issues such as temperature control
and measurement are discussed in some detail.
Learning Objectives:
By the end of this course, you should:
Know which TA techniques are appropriate to measure a variety of materials properties.
Have some practical knowledge of how TA experiments are carried out.
Be able to interpret TA data in order to calculate sample properties.
Equipment for simultaneous thermogravimetry and DTA/DSC
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Synopsis of Course
1. An Introduction to Thermal Analysis Definitions of Thermal Analysis (TA). Properties
commonly studied by TA. Instruments available in the Department. Types of experimental scan.
Reasons to use TA.
2. Differential Thermal Analysis DTA apparatus. DTA scans.
3. Differential Scanning Calorimetry Power-compensated DSC. Heat flux DSC. Temperature
calibration. Measurement of latent heat, specific heat.
4. Other Techniques Thermogravimetric analysis. Dynamic mechanical thermal analysis.
Thin film DSC. Modulated DSC.
5. Examples of TA use Kinetics of phase transformations. Materials science of chocolate.
Polymer identification.
6. Practical Issues for Thermal Analysis Temperature measurement. Furnace materials and
control. Purge gases. Sample preparation.
Additional Resources
Web and computer resources
Thermal Analysis equipment available in the Department is described at:
http://www.msm.cam.ac.uk/industry/PolymerCharacterisationLaboratory.pdf
The TA Instruments website details the state-of-the-art equipment currently on the market
http://www.tainstruments.com/
Useful texts:
M.E. Brown, Introduction to Thermal Analysis (Kluwer, 2001).
R.F. Speyer, Thermal Analysis of Materials (Marcel Dekker Inc., 1994).
T. Hatakeyama and F.X. Quinn, Thermal Analysis (Wiley, 1994).
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1. Introduction
1.1 Definition of Thermal Analysis
The latest definition of Thermal Analysis
Some things worthy of note:
Analysis means more than monitoring. Analysis implies not only the recording of the
data but also any subsequent interpretation.
It is usually the case that a change in the property rather than the property itself which is
studied.
We can only really control the temperature of the environment of the sample, rather than
the sample itself.
1.2 Properties Studied by Thermal Analysis

There are a wide range of properties that may be studied, and each has an associated technique
which can be used:
a) specific heat
b) thermal expansion
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c) weight
d) flow stress
e) viscosity
f) elastic modulus and damping
g) evolved gases
h) phase changes and lattice parameter
Of course, you can measure just about any property as a function of temperature, i.e. electrical
resistivity, magnetic permeability, thermoluminescence. But some techniques (those which have
acquired acronyms) are commonly used and have developed specialised commercial
instrumentation.
Available in this department are:

DSC, DTA, TGA, DTA+TGA, TMA, DTMA, Dielectric TA, Rheometry, dilatometry, EGA, XRD
+ heating
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1.3 Common Types of Experimental Scans
A. Isothermal heat treatment
RT
time
B. Temperature scan
RT
time
The isothermal heat treatment is usually best suited to kinetic studies. It is useful to study things
that happen far away from the equilibrium temperature and hence occur when we hold the
temperature constant
The temperature scan is generally more useful to examine thermodynamic properties. It is useful
to study things that happen near to the equilibrium temperature and hence need us to ramp up from
below the equilibrium temperature to above it in order for the transformation to occur.
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1.4 Why Use Thermal Analysis Techniques?
a) to measure a property of interest, such as specific heat, latent heat or heat of reaction
b) to fingerprint a particular material or substance
c) to assess the high-temperature stability of materials
d) to detect phase transformations
e) fundamental studies of reaction kinetics
This course mainly concentrates on the purely thermal techniques, DTA and DSC.
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2. Differential Thermal Analysis

2.1 DTA Apparatus
This is an older technique which is simple to perform and understand.
The sample of interest (S) and an inert reference (R) are placed in the same furnace and hence are
subject to the same heat treatment. The thermocouples are usually placed directly into the samples
and the difference in temperature is monitored.
Heater
2.2 DTA Scans

Temperature scan for a sample (a pure metal) melting
furnace
reference
sample
Tm
time
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T
Tm
~0
endothermic
Treference
Note that the melting point (Tm) is characterised by the onset of a temperature difference between
the sample and reference. The position of the peak has no significance and is only affected by
factors such as sample size, latent heat of melting and thermal conductivity.
The convention when plotting T is that energy evolved by a transition or reaction is positive.
Hence for the endothermic process shown above, where heat is absorbed by the sample when it
melts, the temperature change is negative.
DTA:
With this technique it is not easy to measure quantitatively the energies involved in transitions. A
different technique is required.
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3. Differential Scanning Calorimetry

3.1 DSC Apparatus
There are two methods of carrying out DSC. Power-compensated DSC is the method usually
discussed in textbooks, though most practical instruments are based on heat-flux DSC. However,
in practice these usually give equivalent experimental results.
3.1.1 Power-compensated DSC (Patented by Perkin-Elmer)

The sample and reference are in separate furnaces, each with a heater coil and a thermocouple. The
aim is to maintain both at the same temperature, even during a thermal event in the sample. The
difference in power supplied to the two furnaces to maintain zero temperature differential between
the sample and the reference is measured.
If we do a temperature scan, the melting peak should be a better-defined shape than for DTA:
power
endothermic
Tm
Treference
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The temperature difference between sample and reference is converted to a differential thermal
power, q (or power), which is supplied to the heaters to maintain the temperature of the sample
and reference at the programmed value.
3.1.2 Heat-flux DSC (developed by TA Instruments)

heating
coil
sample
pan
reference
pan
constantan
chromel/alumel
wires
inert gas
vacuum
thermocouples
chromel wafer
The sample and reference are both within the same furnace and are connected by a low-resistance
heat-flow path. If any difference in temperature develops, heat flows in proportion to that
temperature difference.
DSC :
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3.2 DSC Temperature Calibration
Hence an offset between the thermocouple temperature and the real sample temperature exists and
this is proportional to the heating rate (because the rate of heat flow from heater T). Also if we
increase the mass of the sample, m, T increases.
We can calibrate for this though by measuring the apparent (measured) temperature of a transition
at different heating rates and extrapolating to find what the result would be if the experiment was
done infinitely slowly so that everything was kept in thermal equilibrium.
e.g. for the Curie transition (which always occurs at the same temperature and is independent of
dT/dt).
Tc
(indicated by
thermocouple)
x
x
x
Tc (true)
Tthermocouple = Tsample
0
dT/dt
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We need to calibrate (by shifting the zero of the temperature scale) for every scan which has a
different dT/dt.
A similar process can be carried out for the sample mass:
e.g. for a T-scan melting experiment:
Same dT/dt
power
apparent
Tm
3.3 Measurement of Latent Heat
It is simple to calculate the difference in heat supplied (Q) supplied from the DSC scan.
Q q dt which is the area under the peak in our DSC plot if plotted against time.
For the same sample mass, but different dT/dt the latent heat of melting is independent of
temperature, hence the peak area is constant when plotted on a time axis:
T1
time
T2 > T1
time
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But, we usually plot on a T-axis,

Q q dt q dT .
Peak Area
dt
i.e. Q
hence the peaks at higher dT/dt appear bigger
dT dt
dT
T1
T2 > T1
3.4 Measurement of Heat Capacity

This is determined by a T scan:
time
power
(measured)
time
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This technique works fine for measuring changes in the heat capacity, for example at the Curie
temperature, the glass transition or a structural transition, but one has to be careful if trying to
measure the absolute heat capacity of a sample. The best way to do this is to do a scan with the
sample in place and another scan with nothing in the sample pan. The difference between these
scans should be an accurate measure of the samples heat capacity.
Note than in practice, heat capacity is not a constant even for a given phase.
3.5 Baseline Issues
As well as baseline sloping/curving we have seen that it also usually changes at a structural
transition.
e.g. melting
(T-scan)
power
time
The liquid has a different heat capacity from the solid

baseline shift at transition
This is a problem for kinetic analysis because it isnt clear how to define the area below the curve.
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A simple example is attempting to follow the extent of crystallisation of a glass.
X ~10%
X ~50%
A(T)
The baseline problem does not arise in isothermal scans
A(t)
time
Isothermal scans are therefore best for fundamental analysis, BUT the usable T-range is very
narrow:
If T is too high, the reaction will start during heating.
If T is too low, the signal is difficult to distinguish from the baseline.
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4. Other TA Techniques
4.1 Thermogravimetric Analysis
4.1.1Measurement technique
The weight of the sample is monitored as a function of time or temperature.
Figure from http://www.e-thermal.com/tarsus/tg209_f3_tech_speci.htm
The typical form of TGA curves
measured
net force
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4.1.2 Examples of results oxidation of a metal

Assuming that kinetics is such that x t
Isothermal scans
Temperature scan
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4.2 Dynamic Mechanical Thermal Analysis
Elastically deform the sample:
Measure oscillation frequency
Measure electrical power necessary to maintain the oscillation
This technique is very suitable for studying properties of polymers:
e.g. the glass transition
Tg
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4.3 Nanocalorimetry (Thin Film DSC)
The strips serve as both heaters and temperature sensors. The device is fabricated using
photolithography and etching.
Uses of nano-calorimetry
1. To study the absorption of monolayers onto surfaces
2. In biological studies
3. To perform experiments with ultra-high heating rates (~30,000 K/s)
4. To study the remarkable properties of nm-scaled materials
For more details of this technique, see:

http://allen.mse.uiuc.edu/nanocalorimetry.htm
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4.4 Modulated (or Dynamic) DSC

The heating programme has an imposed sinusoidal variation. Existing hardware can be used and
only new control software is required.
Modulated DSC Heating Profile
time
The normal DSC signal contains:

Specific heat
heat of reaction (crystallisation)
Total heat flow is a combination of reversible and irreversible signals. Using a Fourier transform
analysis of the MDSC signal, the reversible and irreversible components can be separated
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An example of this is use is for an amorphous polymer blend of PET and ABS:
The problem is that the Tg of the ABS is masked as it occurs in the same temperature range as the
Heat Flow (W/g)
crystallisation peak. One option is to do two separate conventional DSC scans, cooling slowly
between them so that for the second scan the polymer is already crystalline (there is no peak
associated with crystallisation):
Second scan after

slow cooling
First heating scan

Temperature (C)
However using modulated DSC, everything can be measured in a single scan by separating the
reversible and irreversible components:
Heat Flow (W/g)
Reversible
TOTAL
Irreversible
Temperature (C)
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5. Practical Uses of Thermal Analysis

5.1 Kinetics
One application of Thermal Analysis is in following phase transformations. Phase transformations:
occur at an interface
are rate controlled by interfacial processes or by long-range diffusion
Example: Planar Interface, Interface control

A practical example of this is the regrowth of Si into a surface layer which has been amorphised
by ion implantation.
A
amorphous Si
single crystal Si
We can measure the activation energy using DSC, because the differential power (the value
plotted vertically on the DSC trace) is a measure of the rate of heat evolution (the crystallisation
process is exothermic) as the planar interface moves.
If HV is the enthalpy of crystallisation (per unit volume), then when the interface proceeds by an
amount dx, the heat (dU) evolved is
hence the rate of heat evolution with time is
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Qgrowth
power H V Av0 exp
RT
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DSC net power (mJ/s)
-1
-2
800
900
1000
T (K)
Hence one could replot this data as an Arrhenius plot [ln (power) vs 1/T] in order to calculate the
energy barrier involved in the growth of crystalline silicon from amorphous silicon.
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5.2 Chocolate
Whilst the taste and appearance of chocolate depends to some extent on its chemical composition,
the microstructure is also crucial. A combination of DSC and XRD as a function of temperature
has shown that there are six different crystalline forms of chocolate around room temperature.
Control of processing parameters to ensure crystallisation of the desired phase is therefore
essential. The DSC measurements below show that the cooling rate from the original melt has a
very significant effect on the melting temperature.
A crucial property of chocolate is that it melts rather sharply at a temperature just below body
temperature. It is the latent heat that makes chocolate (at room temperature) feel cold when you
put it in your mouth.
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5.3 Polymer Identification

There are a number of scenarios in which you may want to identify a polymer. A company which
provides such a service advertises:
Do you want to know what materials your competitors are using?
Do you suspect your materials suppliers are not providing what you asked for?
In addition to industrial espionage and fraud detection there are other uses, such as labeling for
recycling and carrying out tests for plastic explosives.
There are several low-tech identification routes for polymers, such as assessing the density and
appearance but these properties are easily altered by using dyes and fillers. Therefore to be more
confident about identification, it is often necessary to conduct parallel tests.
For simple homopolymers, it is often enough to simply use the peak positions in a DSC scan to
characterize Tg and Tm. e.g. PEEK, a high performance polymer with good mechanical properties
and a melting point around 600 K.
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For polymer blends, the situation is more complex.

A
polystyrene
poly(dimethylphenylene oxide)
These are miscible in all proportions: DSC profiles show a single glass transition temperature,
between 100C and 210C, depending on the relative fractions of the components in the blend
polystyrene
polyisoprene
These are completely immiscible: DSC shows two characteristic glass transition temperatures in
the same temperature ranges as their respective homopolymer blend components.
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6. Experimental Issues for Thermal Analysis

6.1 Temperature Measurement
Measurement of temperature in Thermal Analysis is usually carried out using a thermocouple. If
two dissimilar metals are joined together to make a loop and the junctions of the wires are at
different temperatures, a current will flow.
Metal A
T1
T2
Metal B
This phenomenon is known as the Seebeck effect and is caused by the two metals having differing
free electron densities. Rather than measuring this current, we can interrupt the circuit and measure
the voltage.
A
Tfurnace
Tambient
B
There are a number of common thermocouple types, each identified with a letter. The most
frequently used is K-type, which is made using chromel (a Ni-Cr alloy) and alumel (a Ni-Al
alloy). It is low cost, and can work up to 1200C, but alumel is magnetic and changes properties at
the Curie temperature (354C). K-type thermocouples have a sensitivity of 41 V/C.
For measurements at higher temperatures, other thermocouple types are available, typically
containing Pt and Rh. These are more expensive and have less sensitivity.
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Type
Materials
B
C
E
J
K
N
R
S
T
Platinum30% Rhodium (+)

Platinum 6% Rhodium (-)
W5Re Tungsten 5% Rhenium (+)
W26Re Tungsten 26% Rhenium (-)
Chromel (+)
Constantan (-)
Iron (+)
Constantan (-)
Chromel (+)
Alumel (-)
Nicrosil (+)
Nisil (-)
Platinum 13% Rhodium (+)
Platinum (-)
Platinum 10% Rhodium (+)
Platinum (-)
Copper (+)
Constantan (-)
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Useful Range
1370-1700C
1650-2315C
95-900C
95-760C
95-1260C
650-1260C
870-1450C
980-1450C
-200-350C
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6.2 Furnaces
6.2.1 Furnace materials
Most furnaces are heated by electrical heating elements, and are therefore dependent on resistive
heating. The refractory metal wire, commonly nichrome (Ni-Cr) or Kanthal (Fe-Al-Cr) is wrapped
around a refractory ceramic such as alumina. Ceramic heating elements such as SiC, MoS2 or
stabilized ZrO2 can be used to reach temperatures of 2000C in air.
An alternative furnace design uses infrared radiative heating from tungsten-halogen lamps.
Because the heat can be focused locally on the sample, very fast heating rates, up to 50C/s are
possible.
If sub-ambient temperatures are required, liquid nitrogen (boiling point 77 K) or liquid helium
(4 K) can be used along with resistive heating elements.
6.2.2 Furnace control

Furnace temperature control is essential in order to achieve the desired sample heating profile. To
ensure that the furnace temperature is at the desired temperature, a feedback loop between the
measured temperature and the resistive heating current is required.
The simplest control system one could envisage is a simple on/off control.
The setpoint, Tset, is defined as the desired temperature at some given time.
The furnace temperature therefore oscillates about the setpoint. To prevent high frequency
switching, a dead band is usually introduced such that the system doesnt turn off until T exceeds
Tset by a few degrees and doesnt turn on until the temperature drops a few degrees below Tset.
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The control schedule usually implemented is known as proportional integral derivative (PID), an
algorithm of great general importance in a variety of industrial feedback applications.
Proportional control: Corrective action is applied before the temperature reaches the setpoint by
adjusting the power in proportion to the deviation from the setpoint.
Integral control: The difference between the temperature and the setpoint is summed over time.
This value (the area in the T vs. t plot) is multiplied by some factor and added to the proportion
instruction.
Derivative control: When the system is first turned on and the setpoint ramped from room
temperature, it takes some time for the heat to diffuse to the thermocouple from the heating
elements. During this time, the logic therefore instructs the system to go to full power. As a
consequence, the temperature overshoots the setpoint significantly. To reduce the amount of
overshoot and undershoot when ramping, derivative control dictates that if T < Tset , but is rising
rapidly, the derivative function subtracts power from the control instruction.
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Thus the overall control function is
6.3 Gases
It is often desirable to maintain an inert atmosphere whilst performing a scan.
N2 is often used but the standard (cheap) grade of industrial N2 has a purity around 99.99% (4
nines) and should be dried. Alternatives are Ar and He, though if the purge gas is changed, it is
necessary to recalibrate the temperature and energy scales due to the differences in the thermal
conductivities of the gases.
6.4 Sample Preparation

It is essential that the sample is in good thermal contact with the crucible. This can sometimes be
achieved by melting the sample or raising it above its glass transition temperature, then allowing
to cool before performing a second heating scan. This may not be possible if the first heating scan
is the important one, for example in crystallisation studies. In such cases, it is necessary that the
sample is uniformly and densely packed into the crucible.
A small amount of material is usually desirable in order to minimize temperature gradients within
the sample (around 5-20 mg is usually appropriate). However, it is of course necessary that the
sample material used is representative of the sample as a whole. Therefore for composites or
polymer blends, enough material must be used to ensure this is the case.
Al
Pt
alumina
Ni
Cu
quartz
Question Sheet
Part II Materials Science
C11
C11 Question Sheet

1.
Describe briefly how the DTA technique is performed and sketch a typical DTA plot for
the melting of a pure metal.
Describe briefly how DSC differs from DTA and sketch a typical DSC plot for the
melting of a pure metal.
What are the advantages and disadvantages of the two techniques?
2.
DSC and TGA are useful techniques for monitoring oxidation. Make some simple
assumptions about the thermodynamics and kinetics of oxide growth and state how the
weight is likely to change.
Considering these assumptions, sketch DSC and TGA plots for
i) the isothermal technique
ii) with a constant heating rate.
3.
a) A glassy material is heated at a constant rate in a DSC. Sketch a possible DSC trace,
labelling and explaining briefly the main features, assuming that the trace shows the glass
transition, crystallisation and melting.
b) Which of these phenomena could also be studied in an isothermal DSC, and what
would be the comparative merits of isothermal and continuous-heating DSC for this
purpose?
c) Explain the shape of the DSC peak for the melting of a pure material. Sketch how the
sample and furnace temperature compare during heating. What point on the DSC trace
corresponds to the melting point? What is the relationship between the peak area and the
latent heat of melting of the material?
d) The melting of pure zinc is commonly used for DSC calibration. A 20 mg sample of
zinc is heated at 10 K min-1, and the peak on the DSC trace has an area of 0.371 W K.
From this measurement, what is the latent heat of melting of zinc (in kJ mol-1)?
e) The temperature difference between the onset and the maximum of the melting peak
for the zinc sample is found to be 4.6 K. If the experiment were repeated at the same
heating rate but with a sample of mass 40 mg, what would be the temperature difference
between onset and maximum?
4.
In your handout is DSC data for crystallisation of amorphous silicon developing at a

planar interface, with the rate controlled by atomic jumps at the interface (rather than
long-range diffusion). Use it to calculate the energy barrier, Q, for these atomic jumps.
Question Sheet
5.
Part II Materials Science
C11
The figure below shows schematically an experimental setup which is to be used to

study the melting of a Pb-Sn alloy with the eutectic composition (Tm = 183C).
The equipment consists of:
A tube furnace
2 crucibles (A and B) which will contain different metals
Wires used to make thermocouple measurements (2 long pieces of material C and
1 short piece of material D). These wires are good electrical conductors but are
thin and will not conduct significant amounts of heat.
A voltmeter
The furnace is capable of reaching 1200 C, can be programmed to produce a desired
temperature profile and is fitted with its own thermocouple and temperature readout.
D
A
Furnace
You are provided with pure Au (melting temperature = 1064 C) to use as a reference
material in crucible A. The experiment will study the melting of the alloy in crucible B
by monitoring the measured voltage and the temperature readout of the furnace.
a) What is the name of the TA technique being carried out?
b) Describe in detail the practical considerations of setting up the experiment.
Include in your discussion
furnace settings
the choice of materials for the crucibles A and B and for the thermocouple wires
C and D
how to load and position the crucibles and thermocouple wires
the sensitivity required of the voltmeter
c) Sketch how the furnace setpoint, the furnace temperature (as measured by the furnace
and displayed on its readout) and the actual temperatures of the sample (the alloy) and
reference material would vary with time for a scan in which the alloy melts.
d) Sketch how the voltage measured by the voltmeter would vary with furnace
temperature during this scan. Indicate on your sketch how the features of this plot relate
to the melting temperature of the alloy.
e) Describe how you could perform a number of different scans in order to calibrate this
equipment to measure the melting temperature more accurately.

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II

Natural Sciences Tripos Parts II

Course C11: Thermal Analysis

Equipment for simultaneous thermogravimetry and DTA/DSC

Course C11: Thermal Analysis

Course C11: Thermal Analysis

Some things worthy of note:

1.2 Properties Studied by Thermal Analysis

Course C11: Thermal Analysis

f) elastic modulus and damping

h) phase changes and lattice parameter

Available in this department are:

Course C11: Thermal Analysis

1.3 Common Types of Experimental Scans

A. Isothermal heat treatment

Course C11: Thermal Analysis

1.4 Why Use Thermal Analysis Techniques?

b) to fingerprint a particular material or substance

c) to assess the high-temperature stability of materials

d) to detect phase transformations

e) fundamental studies of reaction kinetics

Course C11: Thermal Analysis

2. Differential Thermal Analysis

This is an older technique which is simple to perform and understand.

2.2 DTA Scans

Course C11: Thermal Analysis

Course C11: Thermal Analysis

3. Differential Scanning Calorimetry

3.1.1 Power-compensated DSC (Patented by Perkin-Elmer)

Course C11: Thermal Analysis

3.1.2 Heat-flux DSC (developed by TA Instruments)

Course C11: Thermal Analysis

3.2 DSC Temperature Calibration

Course C11: Thermal Analysis

3.3 Measurement of Latent Heat

Course C11: Thermal Analysis

But, we usually plot on a T-axis,

3.4 Measurement of Heat Capacity

Course C11: Thermal Analysis

3.5 Baseline Issues

The liquid has a different heat capacity from the solid

Course C11: Thermal Analysis

A simple example is attempting to follow the extent of crystallisation of a glass.

The baseline problem does not arise in isothermal scans

If T is too high, the reaction will start during heating.

If T is too low, the signal is difficult to distinguish from the baseline.

Course C11: Thermal Analysis

Figure from http://www.e-thermal.com/tarsus/tg209_f3_tech_speci.htm

The typical form of TGA curves

Course C11: Thermal Analysis

4.1.2 Examples of results oxidation of a metal

Course C11: Thermal Analysis

4.2 Dynamic Mechanical Thermal Analysis

Elastically deform the sample:

Measure oscillation frequency

Measure electrical power necessary to maintain the oscillation

This technique is very suitable for studying properties of polymers:

e.g. the glass transition

Course C11: Thermal Analysis

4.3 Nanocalorimetry (Thin Film DSC)

3. To perform experiments with ultra-high heating rates (~30,000 K/s)

4. To study the remarkable properties of nm-scaled materials

For more details of this technique, see:

Course C11: Thermal Analysis