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Entropy Trends Parallel Volume: ST ND

The document discusses several key thermal analysis techniques: - Differential scanning calorimetry (DSC) measures the heat absorbed or released during phase transitions like melting or crystallization. - Thermogravimetric analysis (TGA) measures the change in mass of a sample as it is heated, to determine things like decomposition temperature. - Differential thermal analysis (DTA) measures the temperature difference between a sample and an inert reference, to identify exothermic or endothermic transitions. These techniques are useful for characterizing materials and identifying phase changes, degradation temperatures, and other thermal properties and transitions.

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Kahraman Kayacan
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© © All Rights Reserved
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57 views

Entropy Trends Parallel Volume: ST ND

The document discusses several key thermal analysis techniques: - Differential scanning calorimetry (DSC) measures the heat absorbed or released during phase transitions like melting or crystallization. - Thermogravimetric analysis (TGA) measures the change in mass of a sample as it is heated, to determine things like decomposition temperature. - Differential thermal analysis (DTA) measures the temperature difference between a sample and an inert reference, to identify exothermic or endothermic transitions. These techniques are useful for characterizing materials and identifying phase changes, degradation temperatures, and other thermal properties and transitions.

Uploaded by

Kahraman Kayacan
Copyright
© © All Rights Reserved
Available Formats
Download as PPTX, PDF, TXT or read online on Scribd
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Entropy trends parallel volume

S S

Tm T Tg T

H = T S H = 0

1st order transition 2nd order transition


with latent heat no latent heat.
At transition, you have After transition, the
to suddenly put in more rate at which heat must
heat. be supplied changes
Glass Transition Temperature (Tg)
The Tg is important to both morphologies of
thermoplastics
In amorphous materials, it is the temperature at which
the molecules have enough absorbed enough energy and
have moves far enough apart that the material behaves
more rubber-like than glass-like.
The material stretches further when pulled
The material absorbs more impact energy without
fracturing when struck
When the material does fail, it fails in a ductile
manner as opposed to a brittle manner. (If a
material fails in a ductile manner, it yields before it
fails. In a brittle manner, it fails or ruptures before it
yields)
Glass Transition Temperature
(Tg) The sample to the left experienced a brittle
failure
The material did not yield before
failure
The material broke like glass

The sample to the right broke in a ductile


manner
The material yielded (stretched)
before failure
The material behaved more like a
rubber
Glass Transition Temperature (Tg)
Because a semi-crystalline material has a portion of its chain that remains in
an amorphous state, it is also affected by the Tg
- When a S/C material is above its Tg, it can form crystals once it dips
below the Tg crystal formation stops
-The amorphous portions of the chains have enough energy and the
molecules are far enough apart, that the molecules can continue to fold up
and unfold.
- The crystals are more easily pulled apart
- The material is more flexible
Ex. Polyethylene and Polypropylene both have low Tgs. They are
way below room temperature. That is why milk jugs and yogurt
containers are flexible when you take them out of the
refrigerator.
Melting temperature (Tm)
The (Tm) when applied to polymers
suggests not a solid-liquid phase
transition, but a transition from a
crystalline phase to a solid
amorphous phase. Crystalline
melting is only discussed with
thermoplastics, as thermosets will
decompose at high temperatures
rather than melt.
Melt Temperature (Tm)
Amorphous materials dont truly have a Tm. They just continue to soften
more until they behave more like a liquid.
The molecules absorb enough energy and move far enough apart (increase
the free volume) that the material can flow.
When we refer to the melt temperature for amorphous materials, it is usually
the temperature at which we can process it.
Glass transition
temperature (Tg)
The glass transition temperature (Tg)
describes the temperature at which
amorphous polymers undergo a
second order phase transition from a
rubbery, viscous amorphous solid
(fresh spaghetti) to a brittle, glassy
amorphous solid (3 days old
Spaghetti)
Differential Scanning
Calorimetry
Primitive Power Supplies

Thermometers

Sample Reference

Suppose we keep track of RPMs needed to maintain sample and


inert reference at same temperature as both are heated.

Orwe could keep track of current.


1st & 2nd Order DSC Transisions
Differential heat:
the extra heat it takes to get
sample through transitions that
Sample --Reference
the inert reference does
not have.

i i

Tm T Tg T

Real transitions depend on rate of scanning, quality


of thermal contact between sample & container, etc.
Thermal Analysis

Differential Scanning
Thermal Gravimetric
Calorimetry (DSC)
Analysis (TGA)
Measure heat
Measure change in
absorbed or liberated
weight during heating
during heating or
or cooling
cooling

Differential Thermal
analysis (DTA)
- Measure temperature
difference between the
sample and reference.
Thermogravimetric analysis
(TGA)

Monitor change in mass of


sample
Sample: Gas atmosphere:
can be both solid &liquid; CaCO3 CaO + CO2
2-25 mg In vacuum, decompose at ~500C
In air, decompose at ~700C
In CO2, ~900C
Draw tangents of the curve to find the onset and the offset points
Thermal profiles for some common polymers
Differential Thermal analysis (DTA)

Measure sample temperature relative to a reference, for the


same heat transferred

Thermal events: Exothermic event and endothermic event


Reaction/decomposition, Melting, Crystallization, Change in crystal
structure
Glass transition
DTA Combined with TGA

* The area under a DTA


peak is the enthalpy change

Lowering heating rate;


Reducing sample weight

sharper peaks with improved


resolution
It is clear that ABS degrades in two steps. The first step initiates at 180 C
and ends at 480 C and the second step from 480 until 620 C. From the
DTA curve, at least three peaks can be observed overlapping each other for
the first degradation step, this means that the first degradation is not a
simple chemical reaction but several reactions occurring simultaneously.
Suzuki et al. applied thermogravimetry/Fourier transform infrared
(TGA/FTIR) to investigate the degradation of ABS and they found that the
evolution of butadiene commenced at 340 C and styrene at 350 C, while
Differential scanning calorimetric (DSC)
Differential scanning calorimetry or DSC is a thermoanalytical
technique in which the difference in the amount of heat required to
increase
the temperature of a sample and reference are measured as a
function of DTA DSC
temperature.

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