Professional Documents
Culture Documents
theoretical background
Galina Kubyshkina
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Amorphous materials
Typical features
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Materials and their transitions
Phase transitions
phase transitions
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Materials and their transitions
Melting and crystallization
Melting temperature - the temperature under which solid crystalline body has
transition to liquid state
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Materials and their transitions
Glass transition
amorphous solids
Tg
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Materials and their transitions
Rate effect: physical aging
g
in
ol
co
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Aging
Physical and chemical
AGING
chemical physical
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Materials and their transitions
Glass transition, melting, crystallization
crystal region
amorphous
region
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Materials and their transitions
The task
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Standards used
ISO and ASTM Standards
www.iso.ch
www.astm.org
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Thermal Analysis - definition
* International Confederation for Thermal Analysis and Calorimetry (ICTAC)
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Classification of Thermal Analysis methods
By a property under studying
dilatometry
DMA
optical electrical acoustic
pressure
properties properties properties
thermorefractometric analysis
thermospectrometric analysis
thermomicrometric analysis
thermoacoustic analysis
thermoelectrical analysis
Thermally simulated
Alternating current
current analysis
13 analysis
DSC theoretical background
Exothermic and endothermic processes
According to the classification, calorimetry is a technique for determining the quantity of heat
that is either absorbed or released by a substance undergoing a physical or a chemical
change. Such a change alters the internal energy of the substance. At constant pressure, the
internal energy is known as enthalpy, H.
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DSC theoretical background
Enthalpy change between two states
.
The formula clearly shows the relationship between the most
important influential factors, namely, the heating rate and
mass
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DSC theoretical background
DSC measuring principle
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Sample crucibles (vessels)
Factors affecting the choice of a crucible
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DSC calibration
Standard reference material
Standard reference material – a material for which one or more of the thermal properties are sufficiently
homogeneous and well established to be used for the calibration of DSC
apparatus, for the assessment of a measurement method or for assigning
values of materials.
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DSC measurement
Reference specimen
Reference specimen – a known specimen which is usually thermally inactive over the
temperature and time range of interest
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Result of DSC measurement
DSC curve
melting peak
cooling
crystallization peak
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DSC applications
Characteristic temperatures of transitions determination
h/2
Figure 7. DSC curves in the region of a phase transition and the corresponding characteristic temperatures
The temperatures Tmg, Tpm and Tpc are taken as glass transition temperature,
melting temperature and temperature of crystallization respectively.
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DSC applications
Enthalpy of transitions determination
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DSC applications
Enthalpy of transitions determination: problem
Endo.
Considered to have
zero error
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Factors affecting on the result of DSC measurement
factors
input output
material DSC measurement vary
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DSC advantages
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DSC disadvantages
can not really control the rate of experiment (can check with
thermocouple)
dependent on too many parameters
very sensitive to any changes
the result depends a lot from the operator
the procedure of standard parameters evaluation is not
described precise and has lack of thermodynamic background
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DSC use for structure analysis
Indirect method of structure modification observation
Monomodal PA6
Bimodal PA6
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DSC use in quality control
Identification of material
Crystallinity
Purity control
Stability control
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DSC use in quality control
Thermal characteristics of raw material control
polymer
Thermal characteristics measurement
(to fit the requirements of technology)
Identification of polymer
Useful for recycled polymers
additives
Temperature characteristics measurement
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DSC use in quality control
Crystallinity estimation
The properties of polymers are critically affected by their crystallinity: the more
crystalline – the more rigid, strong, brittle it is.
∆Hm 173
Heat flow
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DSC use in quality control
Purity estimation
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Degradation of polymer
Characteristic temperatures of transitions determination
time, years
Polymers are very sensitive to degradation
reactions occurring both during the processing
and during use.
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DSC use in quality control
Oxidation stability estimation
N2 / O2 switch
be clearly seen.
These measurements also allow
thermally, mechanically or
Time
chemically stressed material to
be distinguished from fresh
Figure 13. OIT measurement
material.
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